Other - Fentanyl synthesis

[asub2440]

In a fentanyl synthesis it says to add 10 mmols of NPP. How much is 10 mmols.
Also, it says 10 mmols of ANPP and 12 mmols of Propionyl Chloride. How much IN GRAMS?

Reputation Comments on this post:

fentanyl synthesis is complex, and you dont know what moles are?!?

[Shampoo]

mmols stands for millimoles, or 1/1000 of a mole. A mole is a unit of measurement for chemicals based on their personal molar mass. Multiplying the amount of moles (in the case of NPP, it would be .01) by the molar mass will give the weight in grams.

[Solinari]

Damn, some one would have to pretty fucking sure they know what they are doing to attempt a fentanyl synth, that shit is microgram lethal. I know very little about chemistry, i got a B in high school and i know even less about organic chemistry, but i have to say if someone doesn't know that mmols means millimoles then i don't think they should be attempting a fentanyl synth.

[dr_haldol]

One who isn't able to calculate that shouldn't do any synthesis...

[TAz69x]

dissolve the solid in about 60ml water and 2N NaOH until pH > 12.5, then extract with 3×15ml CH2Cl2.

The Siegfried method also mentions "2N NaOH" as an apparent measurement; I was wondering what kind of measurement this is, and why "then extract with 3x15ml CH2Cl2" is mentioned as 3x15ml instead of "45ml"?

SWIM has no intention of performing this synthesis until SWIM has achieved high marks in upcoming organic chemistry college-level courses, though acquiring proper knowledge all the time is ALWAYS helpful!



PS - this part:
Add to one liter of acetonitrile 3 mole finely powdered potassium carbonate, then add 10 g of PTC catalyst - TBAB or TEBA, or just polyethylene glycol-400. Stir this suspension 15 min at 50-60°C, and then add in little portions your 4-piperidone hydrochloride, watching that the CO2 evolution wasn't too vigorous. Stir another hour at 50-60°C, and then add phenethylbromide dropwise , and stir 15-20 h at mild reflux.
It mentions "little portions of your 4-piperidone hydrochloride" and "phenethylbromide dropwise", but doesn't show a measurement in grams or moles that I can see. Is there any obvious quantity or measurement here that can be inferred?

SWIM thanks you SO MUCH for your help!

[Oneiros]

The "N" signifies normality.

"3x15mL CH2Cl2" means extract with 15mL of DCM, separate the layers, than do it twice more.

The quantity of the reactants would depend on the amount of NPP you want to produce. Clearly, you don't want the amount of Piperidone to exceed the amount of K2CO3.

[TAz69x]

Amazing!, SWIM thanks you so much for your help.

SWIM could then possibly calculate the molar equivalency of piperidone relative to the amount of NPP to be reacted; and perhaps the same with the phenethyl bromide?
Excessive amounts unreacted would be somewhat undesirable, though the highest effective reactive amount without applying excessive quantities is, SWIM assumes, the ideal reaction/quantity to limit adulterants in further intermediary reactions?

Again, SWIM thanks you again for taking the time to donate your knowledge and experience.

[Oneiros]

You could certainly do that.

However, whether piperidone or phenethyl bromide is your limiting reagent, you would want a slight molar excess of the other to ensure that all of it is reacted. Makes it easy to calculate your yields, too. The NPP will be recrystallized or otherwise purified before the next step anyway, so there's no need to worry about leftover reactants.