Hydrolysis of N-formylamphetamine via NaOH+Methanol to obtain Amphetamine freebase

[Bartholomeus]

Forum members

I am looking to obtain the correct information for Hydrolysis of N-formylamphetamine with NaOH solution and Methanol
If anyone have experience and correct data to write ratios of chemicals please post it
The Naoh/methanol Hydrolysis is another method of Hydrolising N-formylamphetamine to obtain amphetamine freebase at the end of this process
one way is with HCL acid which most people know, but the better or more profitable in yield way is with NaOH+Methanol

So I am interested to finally know the correct proportions or ratios of this method
People with experience of this reaction please help

 

[Saul]

..

 

[Saul]

it is not working at all ! even H2o + Methanol also not working .
nothing work ! route after boiling 2 hours with HCl and hydro with NaOH and steam distillation also not work
pH goes always back to 7 after all the water is removed from the freebase .
even when again hydro with NaOH so we have pH 14 and then back separated pH is back 7
and so on .
this last step is wrong in every way and I stay with my earlier explanation that this syntheses needs HCl gas
like describe in the original pdf
after boiling for two hours we need to add HCl GAS 4 minutes to the substance .

 

[Saul]

nobody knows the answer, I get more than 5 different private messages from people that say
after boiling for two hours with HCl if your liquid is not black you did something wrong
yesterday a forum moderator say exact the opposite that the liquid should not be black.

 

[Bartholomeus]

Saul I told you once, now I will tell you for the last time, there is no need for any HCL gas as you are NOT after amphetamine hydrochloride
The n-formylamphetamine which is obtained via leuckart reaction is cleaned and then hydrolysis is performed using Naoh+methanol

I just want to know what are the correct ratios of reagents (which % of Naoh solution, and ratio of n-formylamphetamine/naoh solution/methanol)

So anyone having knowledge of this method please shed some light

 

[Bartholomeus]

Anyone?

 

[tweaker2]

just eyeball the meoh lets say 100gN-formyl use around 200-300ml and add 50% naoh until your ph is highly alkaline 12-14 and then reflux you can add more meoh to the solution after the reflux if needed when you extract the freebase

 

[Bartholomeus]

thanks for answering. say how long to reflux this mixture? what product is obtained after hydrolysation on this way? we get directly amph freebase?
then steam distillation is made directly on this mixture? methanol will also go over with the steam right?

 

[tweaker2]

give it couple hours after the reaction mixture cools and layers seperate extract the upper layer it should be dark in color this contains the amphetamine freebase and methanol distill of methanol and after that do steam distillation

 

[btcboss2022]

Thats correct but you must be very careful with ammonia odor and fumes in the reflux.
In alkaline PH you cant make the last washing with solvent before distilling as in HCL way but not most important because you will make Steam distillation so It will be purified anyway.

 

[花谢花开]

Very good. Based on the solubility, can the free base be extracted from the methanol solution? Evaporate the methylene chloride. Is this alkaline hydrolysis suitable for methamphetamine? Hope to get a reply.

 

[btcboss2022]

Once alkali hydrolisys finished you have 2 options:
- Steam distillation
- Evaporate Methanol, separate layers and extract. Once you have the oil layer isolated made an acid-base washing before drying with anydrous sodium sulfate.

And its suitable for meth too.

 

[sponsor]

so no use off HCl ?

 

[btcboss2022]

In the NaOH way no HCL used.

 

[sponsor]

O.M.G

Finally some good news .

so what we use after N-formy ?

 

[jokerr]

How can I make amphetamine from amphetamine free oil?

 

[w2x3f5]

It is better to use a solution of potassium hydroxide in methanol, which is a stronger alkali than sodium hydroxide; an even better option is cesium carbonate in methanol, it additionally hydrolyzes impurities to an amine.

 

[Saul]

I try it out I order cesium carbonate

 

[btcboss2022]

The problem is that is expensive and you must use a lot to molar ratio equivalence.

 

[Saul]

sodium hydroxide + methanol
is not working at all so Iam gonna try this .
it is a legal product and good prices

 

[w2x3f5]

Better try first potassium hydroxide in methanol, more cheap then cesium

 

[Saul]

I have order it already because I believe in this product