Just a thought here but, around 30 years ago I had cause to dabble in methylamine production at lab scale and above. Something tells me that the way you combined steps (more or less) without isolating/purifying the intermediate and then deciding to use ammonium formate in your final reduction may posibly have resulted in further alkylation of your primary amine. I could be wrong here, as I have not taken the time to map out the potential side reactions with residual first stage intermediates, etc. In your shoes, I probably would have tested for the presence of seconday and/or teriary amines to rule them out and then (if negative for them) probably liberated the free amine from a measured amount of it's salt form as a gas bubbled into an amount of hydrochloric acid calculated to neutralize that specific amount of the salt form of your sample. That would roughly establish the purity of your product and its water content. The presence of ammonium salts can be shown by SLOWLY basifying the sample and seeing if the initial gas being generated suports combustion. Ammonia does not support combustion but methylamine does. In a mixture of ammonium and methylammonium salts, the initial base added will preferentially liberate the weaker base upon the very slow addition of a strong base when the initial gas given off is directed to a flame. I hope that some of these ramblings on my part may be of some assistance to you. I've been retired for nearly a decade but my love for chemistry never dies and its a bit like riding a bicycle. Cheers from America!
@@yorkshirechemist that's what I've been seeing from people who have tried it. I'm mostly curious if I can find a practical use for it. Apparently it's quite explosive.
yeah, that's what Dunstan and Bossi's paper claims, but they don't say which base(s) they used, or how much heat is required you've got to love pre-World War I chemistry papers, they're often brilliantly vague without offering any actual figures or hard experimental evidence for what it's worth, in both this method and the hydroxylamine preparation from chloramine, I smelt nothing other than formaldehyde (which is pretty horrible itself at high temperatures), and I didn't get ill or die, so it's fair to say the amount of HCN formed was negligible
read the english wiki for methylamine and use glycine instead, wich can be conveniently decarboxylated to methylamine with a strong base in water, spontaneously...
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Missed a wide, we have to cook
Just a thought here but, around 30 years ago I had cause to dabble in methylamine production at lab scale and above. Something tells me that the way you combined steps (more or less) without isolating/purifying the intermediate and then deciding to use ammonium formate in your final reduction may posibly have resulted in further alkylation of your primary amine. I could be wrong here, as I have not taken the time to map out the potential side reactions with residual first stage intermediates, etc.
In your shoes, I probably would have tested for the presence of seconday and/or teriary amines to rule them out and then (if negative for them) probably liberated the free amine from a measured amount of it's salt form as a gas bubbled into an amount of hydrochloric acid calculated to neutralize that specific amount of the salt form of your sample. That would roughly establish the purity of your product and its water content. The presence of ammonium salts can be shown by SLOWLY basifying the sample and seeing if the initial gas being generated suports combustion.
Ammonia does not support combustion but methylamine does. In a mixture of ammonium and methylammonium salts, the initial base added will preferentially liberate the weaker base upon the very slow addition of a strong base when the initial gas given off is directed to a flame. I hope that some of these ramblings on my part may be of some assistance to you. I've been retired for nearly a decade but my love for chemistry never dies and its a bit like riding a bicycle. Cheers from America!
This is great, very well explained! I've been intending to investigate methylamine perchorate since there's not a ton of information on it.
I'd imagine it's similar to ammonium perchlorate but less stable since it contains carbon, meaning it could potentially oxidise itself
@@yorkshirechemist that's what I've been seeing from people who have tried it. I'm mostly curious if I can find a practical use for it. Apparently it's quite explosive.
Formaldoxime also decomposes to hcn with base and heat. Nice!
yeah, that's what Dunstan and Bossi's paper claims, but they don't say which base(s) they used, or how much heat is required
you've got to love pre-World War I chemistry papers, they're often brilliantly vague without offering any actual figures or hard experimental evidence
for what it's worth, in both this method and the hydroxylamine preparation from chloramine, I smelt nothing other than formaldehyde (which is pretty horrible itself at high temperatures), and I didn't get ill or die, so it's fair to say the amount of HCN formed was negligible
read the english wiki for methylamine and use glycine instead, wich can be conveniently decarboxylated to methylamine with a strong base in water, spontaneously...
I believe there is a typo in 1:12 slide. The formula shows N-hydroxymethylamine, I think that's supposed to be plain hydroxylamine.
you're right - that is a total brainfart on my part
Is it a spinoff of breaking bad?
no fume hood?
I’ve recently heard. Psilocybin/ lsd can be created in oats in good yields , do you know if true. A fellow Yorkshire guy
no, not in the slightest
psilocybin can be made from genetically modified yeast, but it's not an amateur-friendly procedure