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
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If you ran a leuckart at 140 150 with ammoina formate it would only break down into formamide anyway
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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.
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.
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n-formylamphetamine is a a slightly yellow oily liquid
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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!
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!
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