Complete amphetamine freebase (A-oil) synthesis from P2P(10L scale)

[tweaker2]

this writeup is trash.first of all the temperature with formamide is too low 140-150 sounds about right if u are using ammonium formate but formamide needs higher temp if i remember correctly and secondly N-Formylamphetamine is solid mass not liquid and why would you try to extract it from the reaction mixture completely useless step it only hurts your yields third your hydrolysis is wrong you are using 11l hcl that is insane even if you had 11 kilos of N-Formylamphetamine the amount would be close 2,5 liters of hcl not 11l its 1:1 by molar mass not by volume.why do you make everything so complicating Leuckart is simple reflux hydrolysis and then basify and then steam distill all in same pot so no extractions or solvents are are needed i highly doubt that you have ever done this reaction and if you have your yields are close to zero if you do it as you say.okay merry xmas to all im going to sleep im drunk as hell

 

[Davidrobinson]

If you ran a leuckart at 140 150 with ammoina formate it would only break down into formamide anyway

 

[TheNut22]

I totally agree. Some russian chemists do the Leuckart with ammonium formate even as low temp
as 120 C. I do mine 140-150 C with ammonium formate. With formamide, the temp is around 155-165 C. Even if formate brakes to formamide, there is different temp and mechanism with those two reagents.

 

[UWe9o12jkied91d]

n-formylamphetamine is a a slightly yellow oily liquid

 

[TheNut22]

I have info that tells me the same, that the N-formylamphetamine is light yellow oil.
I don't know why my Leuckart has been failed with 4-5 attempts. And my formyl amine is dark brown,
almost black oil with tiny particles inside, even if I wash it with pure water. Do I burn my reaction mass or something? I heat my clear yellow P2P with ammonium formate first to 100 C (1-2 hours), with luke warm water inside the condenser to drive the water from reaction mixture. Then I gradually raise the temperature to 140-160 C, (16 hours) with very cold water inside my condenser. Can someone tell me what is wrong with here. I use 5 molar equivalents of formate. Now i've done my sixth attempt also with my own made P2P, that had been processed to very clear yellow oil for the first time. I've done the hydrolysis now with KOH/ethanol/water-solution mixture (2 hours). Now I got good amount of oil floating, and extracted to xylene (3 times). I washed it many times with pure water. Now I have it in xylene. If something goes wrong with this also, is it that my formyl derivative was almost black again? Do I burn it or... what?

If someone can help me, I'm really happy and thankful of that! Peace!

 

[TheNut22]

I know I have to get pump to my apparatus, to make vacuum distillations. I have to ask, do normal simple distillation work with A-Oil? If steam distillation will work, like many are sayin, will it work like putting my oil with excess water and heat to 100 C?

 

[Saul]

@ChingShih react in private message to me. I share it with you ;-)
ChingShih say
I do the formamide + formic acid 85% route
But when the leuckart reaction heats up it is directly heated to 160 degrees celsius
it doesnt stay at 100 degrees like you wrote
so i dont know if the people first distill of water and then make the reflux or not
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ansfer

hello I know my friend but you need to take it at 100°c not higher the first hour
this is the only way to get rid off the water leftovers
becouse water boiling point is 100°c
and formic 85% boiling point is 108°c
after 1 hour use reflux

 

[TheNut22]

 

[Davidrobinson]

Is that picture after internal steam distillation?
Did you distill your p2p for 70% yield , or did you use it straight from bmk ?

 

[blackburn]

Yes it is .

I used The P2P immediately after conversion from 5449, i did not distill it.

 

[damakemi]

did you wash the p2p?

 

[blackburn]

@btcboss2022

Hi

what type of equipment can you recommend/ use when distilling the oil?

tthanks

 

[btcboss2022]

Depends on amount to distill, type of distill you need, product...

 

[TheNut22]

My alien friends from Mars makes good oil also. The machine looks almost the same but there is internet, and secure browser, and they watch human porn all night it is disgusting.

 

[damakemi]

I did the Naoh way was wondering if it's possible to distill the oil right after 2-3 hours reflux, after point 2 ?

 

[btcboss2022]

Steam distillation yes.

 

[damakemi]

thanks for answering, can I make a larger amount of formamide and formic acid mix and store it?

 

[btcboss2022]

what you mean exactly?

 

[MisterAnonymous]

Thanks Maestro didn't get it at first now i do

 

[damakemi]

Nice write up, can you tell me please how to prepair the 65% NaOH solution because I'm doing something wrong

 

[btcboss2022]

H2O(1L)+NaOH(650gr) technically is not in this way but will works anyway ;-)

 

[OrgUnikum]

As you say its not so very correct. As what you prepare is regarded to be a 39% solution.
Such concentrations are always by weight say 40% NaOH means 1000 gram solution contain 400 g NaOH and 600g water. But in India a 100% solution is 1/1 by weight NaOH/water, well sometimes. International standard is as told though.

 

[btcboss2022]

I know I know is exactly what I clarified and I only trying to make it simple because it will works anyway.

 

[damakemi]

Thnx for answering, it's looks a whole lot different now. Did you only wash the p2p?

 

[btcboss2022]

Yes bicarbonate solution.

 

[damakemi]

20% ?

 

[btcboss2022]

I always dissolve 1.5kg in around 45L

 

[TheNut22]

sorry

 

[door]

The last result turn it in to crystal ?

 

[damakemi]

I did this the NaOH way. I started with 600gr 5449 and convert that the phosphoric way. I got 375ml p2p then got 430ml N-formyl but ended up with 225ml of a very nice clear base oil after distillation I think the yield is very low. do you got some idea where I could have lost some yield?

 

[TucoSalamanca.]

the subject says optional distillation, is there a problem if I do not follow these instructions?