Oxycodone Extraction

[Woodman]

I need info for a book report.

How do you separate Oxycodone from acetaminophen in percocet 5/325 tabs?

SWIM has tried cold water extraction and ended up with too much leftover material. I'm looking for a more definitive separation.

It's a very detailed book report, so clear, comprehensive, step-by-step instructions would really be appreciated.

[Kemikaru_Tenshu]

Is your book report concerned with cleaning up the results of the previously attempted extraction, or with performing an entirely new one?



~KT

[CrookedEye]

Swim would think a full writeup would be most helpful, especially for others who may have similar interest, but less knowledge on such extractions...

[Sitbcknchill]

He wants a procedure that will work on fresh pills....a procedure that works period....

[Woodman]

An entirely new batch, K/T.

BTW, good to see you back.

[Kemikaru_Tenshu]

Thanks Woodman! It's good to be back.

I'm thinking this one over, and while a (somewhat more ) complicated extraction scheme would definitely do the trick, I'm trying to keep it simple. My current line of thought: 2 stage extraction with water and alcohol, taking advantage of the high solubility of Tylenol in alcohol and the low solubility of Oxycodone HCl in the same, as well as the fact that we already know: the difference in low temp water solubility.

Some experimentation may be necessary....


~KT



Let's see what we have to work with:

[from the Merck]:

************************************************** *******************
Monograph Number: 48
Title: Acetaminophen
CAS Registry Number: 103-90-2
CAS Name: N-(4-Hydroxyphenyl)acetamide
Additional Names: 4¢-hydroxyacetanilide; p-hydroxyacetanilide; p-acetamidophenol; p-acetaminophenol; p-acetylaminophenol; N-acetyl-p-aminophenol; paracetamol

(...)

Molecular Formula: C8H9NO2
Molecular Weight: 151.16.
Percent Composition: C 63.57%, H 6.00%, N 9.27%, O 21.17%

(…)

Properties: Large monoclinic prisms from water, mp 169-170.5°. d421 1.293. uv max (ethanol): 250 nm (e 13800). Very slightly sol in cold water, considerably more sol in hot water. Sol in methanol, ethanol, dimethylformamide, ethylene dichloride, acetone, ethyl acetate. Slightly sol in ether. Practically insol in petr ether, pentane, benzene. LD50 in mice (mg/kg): 338 orally (Starmer), 500 i.p. (Dahlin, Nelson).
Melting point: mp 169-170.5°
Absorption maximum: uv max (ethanol): 250 nm (e 13800)
Density: d421 1.293

-----------------------------------------------------------------------

Monograph Number: 7028
Title: Oxycodone
CAS Registry Number: 76-42-6
CAS Name: (5a)-4,5-Epoxy-14-hydroxy-3-methoxy-17-methylmorphinan-6-one
Additional Names: dihydrohydroxycodeinone; 14-hydroxydihydrocodeinone

(…)

Molecular Formula: C18H21NO4
Molecular Weight: 315.36.
Percent Composition: C 68.55%, H 6.71%, N 4.44%, O 20.29%

(...)

Properties: Long rods from alc, mp 218-220°. Sol in alc, chloroform; nearly insol in ether, water, KOH, NaOH, NH4OH. Does not reduce ammoniacal silver or Fehling's soln.
Melting point: mp 218-220°

Derivative Type: Hydrochloride
CAS Registry Number: 124-90-3
Trademarks: Dinarkon; Eubine (Pharkosar); Eucodal; Eukodal (Merck KGaA); Eutagen; Oxikon; Oxycon; OxyContin (Purdue); Pancodine; Tecodin; Tekodin; Thecodine; Thekodin
Molecular Formula: C18H21NO4.HCl
Molecular Weight: 351.83.
Percent Composition: C 61.45%, H 6.30%, N 3.98%, O 18.19%, Cl 10.08%
Properties: Component of Percodan (Endo) . Long rods from water, dec 270-272°. [a]D20 -125° (c = 2.5). One gram dissolves in 10 ml water. Slightly sol in alc.
Optical Rotation: [a]D20 -125° (c = 2.5)

************************************************** ***

[From rxlist.com]:

Each tablet of Percocet contains:
Acetaminophen: 325 mg
Oxycodone HCl (WARNING: May be habit forming): 5 mg*
*5 mg oxycodone HCl is equivalent to 4.4815 mg oxycodone.
Inactive Ingredients: Microcrystalline cellulose, povidone, pregelatinized starch, stearic acid, and other ingredients.

************************************************** ****************

[Woodman]

Originally Posted by Kemikaru_Tenshu

...I'm thinking this one over, and while a (somewhat more ) complicated extraction scheme would definitely do the trick, ...

I can see doing CWE first. Once that is completed doing alcohol extraction.

I can't see any way to fuse them into a single process.

Nevermind experimenting as that might not be necessary.

Please, if you will, explain the "Somewhat more complicated" extraction which would "definitely do the trick".

As long as it doesn't require fancy lab equipment or hard-to-get chemicals, it might be something I could use to validate my book report.

[Woodman]

bump!

: - )

[daeron]

not into this stuff but it seems that the easiest method would be as follows:
-chill EtOH or MeOH and soak for a short period and than filter
-the rest of the pill mass soak in cold water and decant, repeat
-evap the water and scrape the powder
-soak again in cold alcohol for a short time and filter, dry

id measure the result, i guess the return would be something like 70 to 85% but the result should be pretty pure, since oxy is somewhat soluble in alc, but also it would be interesting to see how much paracetamol you will get from the filtered alcohol and the stuff thats left after CWE.

oh and what are the other inactives? EDIT dumb didnt read the above post.

just thinking outloud:
hmm also if one is into experimenting one could also base it with NaOH, relflux it, or just heat it over a period of an hour or so, and than extract the base with chloroform. i guess that a good deal of paracetamol will hydrolise to get p OH-aniline.....that wont work then

okay maybe its smarter to reflux with H2SO4 or HCl to get pOH-aniline , extract it w toluene or benzene, than do the above water/alc washes.(but than again i dont know absolutely nuffin about oxy and its stability)... freebase it, extract and gass/titrate. dry to evap the formed acid.
course this is just thinking out loud...

[Kemikaru_Tenshu]

Did anyone see my response to this post? Immediately after Woodman's last post above I posted a VERY long response, and it DID show up afterward...

When I have time I will write it up again, but I'd like to know what happened to the last one...


~KT

[Woodman]

I'll look forward to it, K/T.

Please send it in P/M also, and let me know when you find out what happened.

I, too, am interested to know what became of your post.

[godismdma]

Originally Posted by Kemikaru_Tenshu

Thanks Woodman! It's good to be back.

I'm thinking this one over, and while a (somewhat more ) complicated extraction scheme would definitely do the trick, I'm trying to keep it simple. My current line of thought: 2 stage extraction with water and alcohol, taking advantage of the high solubility of Tylenol in alcohol and the low solubility of Oxycodone HCl in the same, as well as the fact that we already know: the difference in low temp water solubility.

Some experimentation may be necessary....


~KT



Let's see what we have to work with:

[from the Merck]:

************************************************** *******************
Monograph Number: 48
Title: Acetaminophen
CAS Registry Number: 103-90-2
CAS Name: N-(4-Hydroxyphenyl)acetamide
Additional Names: 4¢-hydroxyacetanilide; p-hydroxyacetanilide; p-acetamidophenol; p-acetaminophenol; p-acetylaminophenol; N-acetyl-p-aminophenol; paracetamol

(...)

Molecular Formula: C8H9NO2
Molecular Weight: 151.16.
Percent Composition: C 63.57%, H 6.00%, N 9.27%, O 21.17%

(…)

Properties: Large monoclinic prisms from water, mp 169-170.5°. d421 1.293. uv max (ethanol): 250 nm (e 13800). Very slightly sol in cold water, considerably more sol in hot water. Sol in methanol, ethanol, dimethylformamide, ethylene dichloride, acetone, ethyl acetate. Slightly sol in ether. Practically insol in petr ether, pentane, benzene. LD50 in mice (mg/kg): 338 orally (Starmer), 500 i.p. (Dahlin, Nelson).
Melting point: mp 169-170.5°
Absorption maximum: uv max (ethanol): 250 nm (e 13800)
Density: d421 1.293

-----------------------------------------------------------------------

Monograph Number: 7028
Title: Oxycodone
CAS Registry Number: 76-42-6
CAS Name: (5a)-4,5-Epoxy-14-hydroxy-3-methoxy-17-methylmorphinan-6-one
Additional Names: dihydrohydroxycodeinone; 14-hydroxydihydrocodeinone

(…)

Molecular Formula: C18H21NO4
Molecular Weight: 315.36.
Percent Composition: C 68.55%, H 6.71%, N 4.44%, O 20.29%

(...)

Properties: Long rods from alc, mp 218-220°. Sol in alc, chloroform; nearly insol in ether, water, KOH, NaOH, NH4OH. Does not reduce ammoniacal silver or Fehling's soln.
Melting point: mp 218-220°

Derivative Type: Hydrochloride
CAS Registry Number: 124-90-3
Trademarks: Dinarkon; Eubine (Pharkosar); Eucodal; Eukodal (Merck KGaA); Eutagen; Oxikon; Oxycon; OxyContin (Purdue); Pancodine; Tecodin; Tekodin; Thecodine; Thekodin
Molecular Formula: C18H21NO4.HCl
Molecular Weight: 351.83.
Percent Composition: C 61.45%, H 6.30%, N 3.98%, O 18.19%, Cl 10.08%
Properties: Component of Percodan (Endo) . Long rods from water, dec 270-272°. [a]D20 -125° (c = 2.5). One gram dissolves in 10 ml water. Slightly sol in alc.
Optical Rotation: [a]D20 -125° (c = 2.5)

************************************************** ***

[From rxlist.com]:

Each tablet of Percocet contains:
Acetaminophen: 325 mg
Oxycodone HCl (WARNING: May be habit forming): 5 mg*
*5 mg oxycodone HCl is equivalent to 4.4815 mg oxycodone.
Inactive Ingredients: Microcrystalline cellulose, povidone, pregelatinized starch, stearic acid, and other ingredients.

************************************************** ****************

couldnt one extract using alcohol and filter then the left over powder would be mainly oxycodone then use the CWE as a additional step if desidered having the left over liquid mainly containing oxycodone? Or just use the first step leaving a powder that can be thrown into capsules rather than having to drink nasty tasting liquid?

[tinman]

maybe steam distallation is the answer.get a pressure cooker hook a fish tank hose to the little thingamajig on tol of the lid run that dowm to a mason jar say 1 quart or so put yer crushed oxcycone pills in about 1 quart of dh2o and distill till the bottom jar is full.or if an explosion isnt immenent put the pressure cooker on an electric skillet and use about a quart of everclear.whats left in the pressure cooker if watched carefully so it dont burn should be pure oxycodone.just dont use more than 5 or6 mg at a time till u find out how its gonna effect ya,dont wanna wind up dead, or worse in a coma with a pretty nurse changin yer shitty diapers............if yer worried about the metal in the pan from gackin yer product just put a pyrex dish in the bottom, the shit that sticks to the sides of the cooker will be acetmetphine anyway, just trash that crap..................hell swim dont know if this will work but its cheap and worth a try ,any moderator input would be awsomly appreciated ty..........................tinman.........