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  #1  
Old 03-10-2005, 12:12
DJ-666 DJ-666 is offline
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synthetic or "natural" cocaine



Hallo,


does there exist a method to determine if the powder you have in hand is made synthetically or made out of the coca leaves? Cause if someone maybe wants to buy a larger amount SWIM think you should know how its made, or?!


SWIM heard, but he is not sure about it, that there exists a test with ammoniac?!?!


Would be interesting what you think about it, any easy to do procedures?
  #2  
Old 03-10-2005, 13:52
Benga Benga is offline
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can't help you but it gets me wondering how much *synthetic cocaine* is really out there ? I thought it was so expensive and time consuming to make that labs just buy some from official sources like ENACO or others (perhaps the leftovers from soft drink making etc).


often heard the term "vegetable" or natural cocaine as opposed to "synthetic" but I really doubt that that it means anything.


anyway the questions that your stepmothershould ask herselfare rather : how cut is the cocaine and what cuts are used.
  #3  
Old 04-10-2005, 09:02
b16a b16a is offline
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Depends on many variables whether you're getting natural or synthetic, but in my region most of it is produced locally. It is a very complicated and difficult process, but eliminates the risk of being caught smuggling across borders. Synthetic coke characteristics include; hard rocks or chunks, or the opposite - excessive moisture, or a distinct chemical taste. Natural coke is usually rare in parts of the world that are not close to coke producing countries and may be identified by a yellowish colour, and will come in a fine powder form.
  #4  
Old 04-10-2005, 10:54
Benga Benga is offline
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Quote:
Originally Posted by b16a
Depends on many variables whether you're getting natural or synthetic, but in my region most of it is produced locally. It is a very complicated and difficult process, but eliminates the risk of being caught smuggling across borders. Synthetic coke characteristics include; hard rocks or chunks, or the opposite - excessive moisture, or a distinct chemical taste. Natural coke is usually rare in parts of the world that are not close to coke producing countries and may be identified by a yellowish colour, and will come in a fine powder form.

first time I hear this...Do you have any sources on actual illegal synthetic coke and who smuggles it, what kind of networks ? I doubt that southamericans would take so much time to smuggle coke say to europe which is pretty far away if the market was already flooded with synthetic......


texture and tasteissues are not linked to origins but to preparation, packaging and cuts used... very easy to recreate flakes or rocks or fine powder btw...


what you wrote really seems based on cocaine lore rather than on facts
  #5  
Old 04-10-2005, 12:48
DJ-666 DJ-666 is offline
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Hmmm...if this would be right then SWIM has a naturall-synthetical stuff!?!


SWIM thought of anything which should react with ingredients like Succindialdehyde, barium carbonate, methylamine hydrochloride, ammonium chloride, etc...and produces a typical colour.


  #6  
Old 04-10-2005, 18:40
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here's something that might help :


"Due to the crude processing facilities that are used, residual solvents are usually present in illicit cocaine. Because these solvents may be indicative of solvent requirement or if samples are being obtained from a common source the DEA has carried out studies characterizing the volatile components present in cocaine HCl. Prior to 1981 all cocaine samples contained trace levels of acetone and ether. Recent studies indicate that acetone/ether is still preferred for cocaine processing (49% of the samples). However, a decreasing availability of diethyl ether in South America appears to have forced the usage of other solvents such as acetone, methylethylketone (Churchill 1985) and benzene (Kiser 1986). Volatile compounds that are also associated with illicit cocaine samples are the hydrocarbons present in kerosene (alkylbenzenes and hydrocarbons), contaminants of acetone (mesityl oxide and diacetone alcohol), and trans-esterification products from cocaine (methyl benzoate, methyl cinnamate and dimethyltruxillate) (Pettit 1986). (...)





Synthetic" cocaine is identified by the presence of the diastereomers of cocaine (pseudococaine, allococaine or allopseudococaine) or by the d enantiomer of cocaine. Additional contaminants common to most of the synthetic routes are shown in Figure 3. Contaminants that are present in both synthetic and natural cocaines are benzoyl pseudotropine and benzoyltropine."


from


http://www.erowid.org/archive/rhodiu...y/amphetamine- cocaine.impurities.html
  #7  
Old 05-10-2005, 01:34
Benga Benga is offline
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from what I've been reading, it seems that synthetic cocaine is really rare : even pharmaceutical cocaine (ie legal) is made from coca leaves because it's more cost effective.


Seems what people call "synthetic" coke is either cocaine with certain cutting agents which makes one think that the product is "less natural" or simply not cocaine (amphetamines for instance)


Edited by: benga
  #8  
Old 06-10-2005, 11:44
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Quote:
Originally Posted by benga

Quote:
Originally Posted by b16a
Depends on many variables whether you're getting natural or synthetic, but in my region most of it is produced locally. It is a very complicated and difficult process, but eliminates the risk of being caught smuggling across borders. Synthetic coke characteristics include; hard rocks or chunks, or the opposite - excessive moisture, or a distinct chemical taste. Natural coke is usually rare in parts of the world that are not close to coke producing countries and may be identified by a yellowish colour, and will come in a fine powder form.

first time I hear this...Do you have any sources on actual illegal synthetic coke and who smuggles it, what kind of networks ? I doubt that southamericans would take so much time to smuggle coke say to europe which is pretty far away if the market was already flooded with synthetic......


texture and taste*issues are not linked to origins but to preparation, packaging and cuts used... very easy to recreate flakes or rocks or fine powder btw...


what you wrote really seems based on cocaine lore rather than on facts
Let's just PRETEND that SWIM has 'friends' who have been the sole producers/distributors of synthetic coke for the area where SWIM resides. Of course I can't physically show you the process first hand, however I can provide you with the following:

The basic formula for cocaine starts by purchasing or making tropinone, converting the tropinone into 2-carbomethoxytropinone (also known as methyl-tropan-3-one-2-carboxylate), reducing this to ecgonine, and changing that to cocaine.

Sounds easy? It really is not very simple, but with new drug policies, cracking down on all of the drug smuggling at the borders, this synthetic cocaine may be the source of the future.

This synthesis is certainly worth performing with the high prices that cocaine is now commanding. As usual, I will start with the precursors and intermediates leading up to the product.

Succindialdehyde. This can be purchased, too. 23.2 g of succinaldoxime powder in 410 ml of 1 N sulfuric acid and add dropwise with stirring at 0j a solution of 27.6 g of sodium nitrite in 250 ml of water over 3 hours.

After the addition, stir and let the mixture rise to room temp for about 2 hours, taking care not to let outside air into the reaction. Stir in 5 g of Ba carbonate and filter.

Extract the filtrate with ether and dry, evaporate in vacuo to get the succindialdehyde.

This was taken from JOC, 22, 1390 (1957).
To make succinaldoxime, see JOC, 21, 644 (1956).



Complete Synthesis of Succindialdehyde. JACS, 68, 1608 (1946).

In a 2 liter 3 necked flask equipped with a stirrer, reflux condenser, and an addition funnel, is mixed 1 liter of ethanol, 67 g of freshly distilled pyrrole, and 141 g of hydroxylamine hydrochloride.

Heat to reflux until dissolved, add 106 g of anhydrous sodium carbonate in small portions as fast as reaction will allow. Reflux for 24 hours and filter the mixture.

Evaporate the filtrate to dryness under vacuo. Take up the residue in the minimum amount of boiling water, decolorize with carbon, filter and allow to recrystallize in refrigerator.

Filter to get product and concentrate to get additional crop. Yield of succinaldoxime powder is a little over 40 g, mp is 171-172j.



5.8 g of the above powder is placed in a beaker of 250 ml capacity and 54 ml of 10% sulfuric acid is added.

Cool to 0j and add in small portions of 7 g of sodium nitrite (if you add the nitrite too fast, nitrogen dioxide fumes will evolve).

After the dioxime is completely dissolved, allow the solution to warm to 20j and effervescence to go to completion. Neutralize the yellow solution to litmus by adding small portions of barium carbonate.

Filter off the barium sulfate that precipitates. The filtrate is 90% pure succindialdehyde and is not purified further for the reaction to create tropinone. Do this procedure 3 more times to get the proper amount for the next step, or multiply the amounts given by four and proceed as described above.

Take the total amount of succinaldehyde (obtained from 4 of the above syntheses combined) and without further treatment or purification (this had better be 15.5 g of succindialdehyde) put into an Erlenmeyer flask of 4-5 liters capacity.

Add 21.6 g of methylamine hydrochloride, 46.7 g of acetonedicarboxylic acid, and enough water to make a total volume of 2 liters. Adjust the pH to 8-10 by slowly adding a saturated solution of disodium phosphate.

The condensate of this reaction (allow to set for about 6 days) is extracted with ether, the ethereal solution is dried over sodium sulphate and distilled, the product coming over at 113j at 25 mm of pressure is collected.

Upon cooling, 14 g of tropinone crystallizes in the pure state. Tropinone can also be obtained by oxidation of tropine with potassium dichromate, but I could not find the specifics for this operation.



2-Carbomethoxytropinone. A mixture of 1.35 g of sodium methoxide (this is sodium in a minimum amount of methanol), 3.5 g of tropinone, 4 ml of dimethylcarbonate and 10 ml of toluene is refluxed for 30 min. Coo] to 0j and add 15 ml of water that contains 2.5 g of ammonium chloride.

Extract the solution after shaking with four 50 ml portions of chloroform, dry, evaporate the chloroform in vacuo. Dissolve the oil residue in 100 ml of ether, wash twice with a mixture of 6 ml of saturated potassium carbonate and three ml of 3 N KOH.

Dry and evaporate in vacuo to recover the unreacted tropinone. Take up the oil in a solution of aqueous ammonium chloride and extract with chloroform, dry, and evaporate in vacuo to get an oil.

The oil is dissolved in hot acetone, cool, and scratch inside of flask with glass rod to precipitate 2- carbomethoxytropinone. Recrystallize 16 g of this product in 30 ml of hot methyl acetate and add 4 ml of cold water and 4 ml of acetone. Put in freezer for 2l/2 to 3 hours.

Filter and wash the precipitate with cold methyl acetate to get pure product.



Methylecgonine. 0.4 mole of tropinone is suspended in 80 ml of ethanol in a Parr hydrogenation flask (or something that can take 100 psi and not react with the reaction, like stainless steel or glass).

10 g of Raney Nickle is added with good agitation (stirring or shaking) followed by 2- 3 ml of 20% NaOH solution.

Seal vessel, introduce 50 psi of hydrogen atmosphere (after flushing vessel with hydrogen) and heat to 40-50j.

After no more uptake of hydrogen (pressure gauge will hold steady after dropping to its lowest point) bleed off pressure and filter the nickle off, rinse out bottle with chloroform and use this rinse to rinse off the nickle while still on the filter paper. Make the filtrate basic with KOH after cooling to 10j.

Extract with chloroform dry, and evaporate the chloroform in vacuo to get an oil. Mix the oil plus any precipitate with an equal volume of dry ether and filter.

Add more dry ether to the filtrate until no more precipitate forms, filter and add to the rest of the precipitate. Recrystallize from isopropanol to get pure methylecgonine. Test for activity.

If active, skip down to the step for cocaine. If not active, proceed as follows. Stir with activated carbon for 30 min, filter, evaporate in vacuo, dissolve the brown liquid in methanol, and neutralize with 10% HCI acid in dry ether.

Evaporate the ether until the two layers disappear, and allow to stand for 2 hours at 0j to precipitate the title product. There are many ways to reduce 2-carbomethoxytropinone to methylecgonine.

I chose to design a Raney Nickle reduction because it is cheap and not as suspicious as LAH and it is much easier than zinc or sodium amalgams.



Cocaine. 4.15 g of methylecgonine and 5.7 g of benzoic anhydride in 150 ml of dry benzene are gently refluxed for 4 hours taking precaution against H20 in the air (drying tube).

Cool in an ice bath, acidify carefully with hydrochloric acid, dry, and evaporate in a vacuum to get a red oil which is treated with a little portion of isopropanoi to precipitate cocaine.

As you can see, this is quite a chore. The coca leaves give ecgonine, which as you can see, is only a Jump away from cocaine.

If you can get egconine, then dissolve 8l/2 g of it in 100 ml of ethanol and pass (bubble) dry HC1 gas through this solution for 30 min. Let cool to room temp and let stand for another 11/2 hours. Gently reflux for 30 min and evaporate in vacuo.

Basify the residue oil with NaOH and filter to get 8.4 g of methylecgonine, which is converted to cocaine as in the cocaine step above.



Below is given a somewhat easier method of producing tropinone by the general methods of Willstatter, who was instrumental in the first synthetic production of cocaine and several other alkaloids. After reviewing this method, I found it to be simpler than the above in many respects.

Tropinone. 10 g of pyrrolidinediethyl diacetate are heated with 10 g of cymene and 2 g of sodium powder, the reaction taking place at about 160j. During the reaction (which is complete in about 10 min) the temp should not exceed 172j.

The resulting reaction product is dissolved in water, then saturated with potassium carbonate, and the oil, which separates, is boiled with dilute sulfuric acid. 2.9 g of tropinone picrate forms and is filtered.



Here are two more formulas devised by Willstatter that produce tropinone from tropine. Take note of the yield differences.

Tropinone. To a solution of 25 g tropine, dissolved in 10 times its weight of 20% sulfuric acid are added 25 g of a 4% solution of potassium permanganate in 2 or 3 g portions over 45 min while keeping the temp at 10-12j.

The addition of permanganate will cause heat (keep the temp 10-12j) and precipitation of manganese dioxide. The reaction mixture is complete in I hour.

A large excess of NaOH is added and the reaction is steam distilled until I liter of distillate has been collected.

The tropinone is isolated as the dibenzal compound by mixing the distillate with 40 g of benzaldehyde in 500 cc of alcohol and 40 g of 10% sodium hydroxide solution. Let stand several days to get dibenzaltropinone as yellow needles. Yield: 15.5 g, 28%. Recrystallize from ethanol to purify.



Tropinone. A solution of 12 g of chromic acid in the same amount of water (12 g) and 60 g of glacial acetic acid is added dropwise with stirring over a period of 4 hours to a solution of 25 g of tropine in 500 cc of glacial acetic acid that has been warmed to 60-70j and is maintained at this temp during the addition.

Heat the mixture for a short time on a steam bath until all the chromic acid has disappeared, cool and make strongly alkaline with NaOH. Extract with six 500 cc portions of ether and evaporate the ether in vacuo to get an oil that crystallizes readily.

Purify by converting to the picrate or fractionally distill, collecting the fraction at 224-225j at 714 mm vacuo.

The tropinones can be used in the above formula (or in a formula that you have found elsewhere) to be converted to cocaine. Remember to recrystallize the 2-carbomethoxytropinone before converting to methylecgonine.

In closing, the preceding is widely used in areas (as I said) that are NOT in close proximity to 'natural' cocaine producing countries.
  #9  
Old 06-10-2005, 13:07
Benga Benga is offline
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I know the formula, B16,and that cocaine can and has been synthesized in clandestine labs, especially in canada where labs have been dismantled.


you're not getting my point, i'm not saying that cocaine synthesis is not possible, or that it doesn't happen.


However, drug enforcement sources tend to point that in europe (remember the original poster is in germany)at least cocaine seized or analysed is seldom of synthetic origin, originwhich can be determined not by looks but by traces of solvents used and contamination.


However, "synthetic" versus "natural" coke is a common marketing device, and different effects of cocaine, especially induced by active cutting agents, are attributed to origin of cocaine. This is just not true, at least in europe.


the "synthetic cocaine" issue started in the Reagan era, if you read up on it you can see that it was the big scare, was synthetic cocaine going to flood the continent etc...didn't happen yet, for numerous reason of which price and technicity are among the most important... with the actual south american producing prices, it's more simple to import than synthesize.


now i'm not saying there's no "synthetic cocaine" out there, but that it's pretty low key compared to leaf based, especially in europe.


and as for determination of origin by looks, andwithout chemical analysis, no chance
  #10  
Old 06-10-2005, 17:01
DJ-666 DJ-666 is offline
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Oh oh oh oh oh oh...my easy question leaves unanswered i think!


  #11  
Old 07-10-2005, 11:03
b16a b16a is offline
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My reply to the original thread only states SOME common characteristics of the two types of cocaine. In Canada, the synthetic type is prevalent and can be easily identified as such by the traits that I mentioned.
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Old 07-10-2005, 12:32
DJ-666 DJ-666 is offline
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Yes yes, its clear that the synthetic has other traits than the "natural", and due to this was my original question, only to identify one of the ingredients which were used in the synthesis via an easy to do ex post reaction with a special substance.


As i heared there exists something which can be easily handled.


Hope that anyone undertands what i mean with my school english
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Old 08-10-2005, 14:54
Benga Benga is offline
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Quote:
Originally Posted by DJ-666


Yes yes, its clear that the synthetic has other traits than the "natural", and due to this was my original question, only to identify one of the ingredients which were used in the synthesis via an easy to do ex post reaction with a special substance.


As i heared there exists something which can be easily handled.


Hope that anyone undertands what i mean with my school english


yes i'm sure it can be done, i guess you would have to find the right reactive to identify contamination traces, depending on the contaminant present you could identify the Hcl's origin (test diastereomers of cocaine (pseudococaine, allococaine or allopseudococaine) or by the d enantiomer of cocaine which identify synth. cocaine)but for most purposes, wouldn't it seems more logical, and simple, to test the cocaine's actualpurity (burning point for instance), and identifying cutting agents ?
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Old 16-01-2006, 06:15
newguy22 newguy22 is offline
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Difference in potency between synthetic and naturally derived cocaine?

hello.
swim was just wondering igf there is a difforence in potency between cocaine made from the coca plant and synthetic cocaine?
is it possible to tell the diff between the two?
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Old 18-01-2006, 05:54
b16a b16a is offline
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Long story (kinda) short, natural coke is usually fairly consistent. Synthetic, on the other hand, can be manufactured to varying degrees of potency. If the manufacturer takes the time to do it properly, it's possible for the product to be more potent than the natural stuff. However, by the time it reaches us little people, it's more likely that it's been stepped on more than a few times. Commonly, the difference between the two can be identified by colour, taste, and form. Without any cutting agents, synthetic is usually pure white, very bitter tasting, medicinal scented, and crystaline or crunchy/rocky.
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Old 18-01-2006, 13:25
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Cocaine, whether derived from a natural source or from a chemical reaction, is cocaine. There would be no difference whatsoever. Just as there is no difference in sodium chloride-salt-derived from sea water or from reacting sodium metal with chlorine gas.

On the other hand, synthetic cocaine is almost never heard of. The synthesis is ridiculously complex and expensive. At least it was the last time I looked into it. Maybe someone has come up with a newer method.
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Old 18-01-2006, 14:08
Benga Benga is offline
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Quote:
Originally Posted by b16a
Commonly, the difference between the two can be identified by colour, taste, and form. Without any cutting agents, synthetic is usually pure white, very bitter tasting, medicinal scented, and crystaline or crunchy/rocky.
and rather rare...

there's already been a thread on this issue here

http://www.drugs-forum.com/forum/showthread.php?t=12207

still don't really agree with this description of a "looks and taste identification" , as stated before...
but then who's seen uncut cocaine, natural or synthetic, to compare ? maybe SWIY has but SWIM certainly hasn't. If you are SWIY is one lucky SWIY...

if you're dealing with cut cocaine products, like most of the people who don't happen to personally know manufacturers of synth or natural cocaine (not that difficult maybe, some people do manage to produce bathtub eightballs of over 80% pure leaf based cocaine after all) or first hand importers,

then one should point out that taste and consistency, appearance comes mostly from the cutting agents (active or inactive) used, and from the way the cocaine has been handled, smuggled, processed (into rock form, into flakes etc etc... there's books on these processes like Gottlieb's "pleasures of cocaine" from the 70's...).

Synthetic cocaine is expensive and difficult to manufacture, and in this respect rather rare, really. Not saying it doesn't exist but those south american exports *do* end up somewhere.
Really this whole "natural" vs "synthetic" cocaine is more cocaine-lore and dealer selling arguments than anything else....

Here is a description of one way cocaine origin was determined, which is more reliable than trying to determine origin by appearance or taste or whatever...


"Due to the crude processing facilities that are used, residual solvents are usually present in illicit cocaine. Because these solvents may be indicative of solvent requirement or if samples are being obtained from a common source the DEA has carried out studies characterizing the volatile components present in cocaine HCl. Prior to 1981 all cocaine samples contained trace levels of acetone and ether. Recent studies indicate that acetone/ether is still preferred for cocaine processing (49% of the samples). However, a decreasing availability of diethyl ether in South America appears to have forced the usage of other solvents such as acetone, methylethylketone (Churchill 1985) and benzene (Kiser 1986). Volatile compounds that are also associated with illicit cocaine samples are the hydrocarbons present in kerosene (alkylbenzenes and hydrocarbons), contaminants of acetone (mesityl oxide and diacetone alcohol), and trans-esterification products from cocaine (methyl benzoate, methyl cinnamate and dimethyltruxillate) (Pettit 1986). (...)

Synthetic" cocaine is identified by the presence of the diastereomers of cocaine (pseudococaine, allococaine or allopseudococaine) or by the d enantiomer of cocaine. Additional contaminants common to most of the synthetic routes are shown in Figure 3. Contaminants that are present in both synthetic and natural cocaines are benzoyl pseudotropine and benzoyltropine."

from

http://www.erowid.org/archive/rhodiu...mpurities.html

b

Last edited by Benga; 18-01-2006 at 15:05.
  #18  
Old 16-06-2006, 15:45
WrtngCocaineTutorial WrtngCocaineTutorial is offline
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the synthetic / "natural" cocaine thread

Adma Gottlieb writes "cocaine may also be synthsized. Detailed instructions for doind so are given in Basic Drug Manufacture, a Twenties Century Alchemist publication.

Anyone heard of/tried synthetic coke?

Last edited by Benga; 21-09-2007 at 14:49.
  #19  
Old 16-06-2006, 17:18
matti_2003 matti_2003 is offline
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From what Swim gathers its pretty rare because the synthesis is quite complex. There was a thread about it a while ago
http://www.drugs-forum.com/forum/showthread.php?t=15240
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Old 16-06-2006, 17:32
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Thanks Matti!

Thanks! Appriciate it
  #21  
Old 16-06-2006, 18:20
rxbandit Gold member rxbandit is offline
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i know theres a synthetic route to cocaine using atropine.
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Old 16-06-2006, 19:06
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what do you mean?

having atoripine as a base would make it easier?
  #23  
Old 16-06-2006, 19:45
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The basic formula for cocaine starts by purchasing or making tropinone, converting the tropinone into 2- carbomethoxytropinone (also known as methyl-tropan-3-one-2-carboxylate), reducing this to ecgonine, and changing that to cocaine. Sounds easy? It really is not very simple, but with Reagan's new drug policies, cracking down on all of the drug smuggling at the borders, this synthetic cocaine may be the source of the future. This synthesis is certainly worth performing with the high prices that cocaine is now commanding. As usual, I will start with the precursors and intermediates leading up to the product.
Succindialdehyde
This can be purchased, too. 23.2 g of succinaldoxime powder in 410 ml of 1 N sulfuric acid and add dropwise with stirring at 0C a solution of 27.6 g of sodium nitrite in 250 ml of water over 3 hours. After the addition, stir and let the mixture rise to room temp for about 2 hours, taking care not to let outside air into the reaction. Stir in 5 g of Ba carbonate and filter. Extract the filtrate with ether and dry, evaporate in vacuo to get the succindialdehyde. This was taken from JOC, 22, 1390 (1957). To make succinaldoxime, see JOC, 21, 644 (1956).
Complete Synthesis of Succindialdehyde
JACS, 68, 1608 (1946)
In a 2 liter 3 necked flask equipped with a stirrer, reflux condenser, and an addition funnel, is mixed 1 liter of ethanol, 67 g of freshly distilled pyrrole, and 141 g of hydroxylamine hydrochloride. Heat to reflux until dissolved, add 106 g of anhydrous sodium carbonate in small portions as fast as reaction will allow. Reflux for 24 hours and filter the mixture. Evaporate the filtrate to dryness under vacuo. Take up the residue in the minimum amount of boiling water, decolorize with carbon, filter and allow to recrystallize in refrigerator. Filter to get product and concentrate to get additional crop. Yield of succinaldoxime powder is a little over 40 g, mp is 171-172C.
5.8 g of the above powder is placed in a beaker of 250 ml capacity and 54 ml of 10% sulfuric acid is added. Cool to 0C and add in small portions of 7 g of sodium nitrite (if you add the nitrite too fast, nitrogen dioxide fumes will evolve). After the dioxime is completely dissolved, allow the solution to warm to 20C and effervescence to go to completion. Neutralize the yellow solution to litmus by adding small portions of barium carbonate. Filter off the barium sulfate that precipitates. The filtrate is 90% pure succindialdehyde and is not purified further for the reaction to create tropinone. Do this procedure 3 more times to get the proper amount for the next step, or multiply the amounts given by four and proceed as described above.
Take the total amount of succinaldehyde (obtained from 4 of the above syntheses combined) and without further treatment or purification (this had better be 15.5 g of succindialdehyde) put into an Erlenmeyer flask of 4-5 liters capacity. Add 21.6 g of methylamine hydrochloride, 46.7 g of acetonedicarboxylic acid, and enough water to make a total volume of 2 liters. Adjust the pH to 8-10 by slowly adding a saturated solution of disodium phosphate. The condensate of this reaction (allow to set for about 6 days) is extracted with ether, the ethereal solution is dried over sodium sulphate and distilled, the product coming over at 113C at 25 mm of pressure is collected. Upon cooling, 14 g of tropinone crystallizes in the pure state. Tropinone can also be obtained by oxidation of tropine with potassium dichromate, but I could not find the specifics for this operation.
2-Carbomethoxytropinone
A mixture of 1.35 g of sodium methoxide (this is sodium in a minimum amount of methanol), 3.5 g of tropinone, 4 ml of dimethylcarbonate and 10 ml of toluene is refluxed for 30 min. Cool to 0C and add 15 ml of water that contains 2.5 g of ammonium chloride. Extract the solution after shaking with four 50 ml portions of chloroform, dry, evaporate the chloroform in vacuo. Dissolve the oil residue in 100 ml of ether, wash twice with a mixture of 6 ml of saturated potassium carbonate and three ml of 3 N KOH. Dry and evaporate in vacuo to recover the unreacted tropinone. Take up the oil in a solution of aqueous ammonium chloride and extract with chloroform, dry, and evaporate in vacuo to get an oil. The oil is dissolved in hot acetone, cool, and scratch inside of flask with glass rod to precipitate 2-carbomethoxytropinone. Recrystallize 16 g of this product in 30 ml of hot methyl acetate and add 4 ml of cold water and 4 ml of acetone. Put in freezer for 2.5-3 hours. Filter and wash the precipitate with cold methyl acetate to get pure product.
Methylecgonine
0.4 mole of tropinone is suspended in 80 ml of ethanol in a Parr hydrogenation flask (or something that can take 100 psi and not react with the reaction, like stainless steel or glass). 10 g of Raney Nickle is added with good agitation (stirring or shaking) followed by 2-3 ml of 20% NaOH solution. Seal vessel, introduce 50 psi of hydrogen atmosphere (after flushing vessel with hydrogen) and heat to 40-50C. After no more uptake of hydrogen (pressure gauge will hold steady after dropping to its lowest point) bleed off pressure and filter the nickle off, rinse out bottle with chloroform and use this rinse to rinse off the nickle while still on the filter paper. Make the filtrate basic with KOH after cooling to 10C. Extract with chloroform dry, and evaporate the chloroform in vacuo to get an oil. Mix the oil plus any precipitate with an equal volume of dry ether and filter. Add more dry ether to the filtrate until no more precipitate forms, filter and add to the rest of the precipitate. Recrystallize from isopropanol to get pure methylecgonine. Test for activity. If active, skip down to the step for cocaine. If not active, proceed as follows. Stir with activated carbon for 30 min, filter, evaporate in vacuo, dissolve the brown liquid in methanol, and neutralize with 10% HCl acid in dry ether. Evaporate the ether until the two layers disappear, and allow to stand for 2 hours at 0C to precipitate the title product. There are many ways to reduce 2-carbomethoxytropinone to methylecgonine. I chose to design a Raney Nickle reduction because it is cheap and not as suspicious as LAH and it is much easier than zinc or sodium amalgams.
Cocaine
4.15 g of methylecgonine and 5.7 g of benzoic anhydride in 150 ml of dry benzene are gently refluxed for 4 hours taking precaution against H2O in the air (drying tube). Cool in an ice bath, acidify carefully with hydrochloric acid, dry, and evaporate in a vacuum to get a red oil which is treated with a little portion of isopropanoi to precipitate cocaine.
As you can see, this is quite a chore. The coca leaves give ecgonine, which as you can see, is only a jump away from cocaine. If you can get egconine, then dissolve 8.5 g of it in 100 ml of ethanol and pass (bubble) dry HCl gas through this solution for 30 min. Let cool to room temp and let stand for another 1.5 hours. Gently reflux for 30 min and evaporate in vacuo. Basify the residue oil with NaOH and filter to get 8.4 g of methylecgonine, which is converted to cocaine as in the cocaine step above.
Below is given a somewhat easier method of producing tropinone by the general methods of Willstatter, who was instrumental in the first synthetic production of cocaine and several other alkaloids. After reviewing this method, I found it to be simpler than the above in many respects.
Tropinone
10 g of pyrrolidinediethyl diacetate are heated with 10 g of cymene and 2 g of sodium powder, the reaction taking place at about 160C. During the reaction (which is complete in about 10 min) the temp should not exceed 172C. The resulting reaction product is dissolved in water, then saturated with potassium carbonate, and the oil, which separates, is boiled with dilute sulfuric acid. 2.9 g of tropinone picrate forms and is filtered.
Here are two more formulas devised by Willstatter that produce tropinone from tropine. Take note of the yield differences.
Tropinone
To a solution of 25 g tropine, dissolved in 10 times its weight of 20% sulfuric acid are added 25 g of a 4% solution of potassium permanganate in 2 or 3 g portions over 45 min while keeping the temp at 10-12C. The addition of permanganate will cause heat (keep the temp 10-12C) and precipitation of manganese dioxide. The reaction mixture is complete in I hour. A large excess of NaOH is added and the reaction is steam distilled until I liter of distillate has been collected. The tropinone is isolated as the dibenzal compound by mixing the distillate with 40 g of benzaldehyde in 500 cc of alcohol and 40 g of 10% sodium hydroxide solution. Let stand several days to get dibenzaltropinone as yellow needles. Yield: 15.5 g, 28%. Recrystallize from ethanol to purify.
Tropinone
A solution of 12 g of chromic acid in the same amount of water (12 g) and 60 g of glacial acetic acid is added dropwise with stirring over a period of 4 hours to a solution of 25 g of tropine in 500 mL of glacial acetic acid that has been warmed to 60-70C and is maintained at this temp during the addition. Heat the mixture for a short time on a steam bath until all the chromic acid has disappeared, cool and make strongly alkaline with NaOH. Extract with six 500 mL portions of ether and evaporate the ether in vacuo to get an oil that crystallizes readily. Purify by converting to the picrate or fractionally distill, collecting the fraction at 224-225C at 714 mm vacuo.
The tropinones can be used in the above formula (or in a formula that you have found elsewhere) to be converted to cocaine. Remember to recrystallize the 2-carbomethoxytropinone before converting to methylecgonine.


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Great write-up, read it before years ago.
Very good and useful post
  #24  
Old 16-06-2006, 19:47
rxbandit Gold member rxbandit is offline
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atropine is synthesized by reacting tropine with tropic acid. i remember seeing a full synthesis from nightshade to cocaine but it looks like its been taken down for whatever reason.
  #25  
Old 16-06-2006, 20:03
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If you read the above synthisis, and did not understand every word of it - you are not capable of performing it. Sorry - but that's the truth.

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