Yeah but you can only reduce so much by adding all at once, you can’t expect to reduce almost 300g of raw material in one go.If you go back in the thread i think the guy that says this even says in small scale conditions, but maybe im misremembering.
I *****ed around with 25g of borohydride a few...
Respect the procedure next time, especially if it’s the first time you’re doing itor you’re unexperienced.It says dropwise.Do you have external cooling? Ice bath works great.
https://bb.expert/threads/leuckart-amination-of-1-phenyl-2-propanone-smale-scale.47/
Here you go.But why go trough all this trouble and low yield when you can just go the fenyl-two-nitropropene way? Starting from the ketone is more advantageous for metilamphetamine, I believe
I don’t know this reaction personally but from what you are describing maybe you can try less cooling? Do a micro synth and see what happens with temperatures increased a little.
I think you are correct.Distill crude product -> Get pure product -> Dillute with cold aceton -> Gas the aceton solution.
I don’t have first hand experience working up md but this is the way it makes sense the most.
I would not play around with that reaction if it were me.Besides you get a mix of 4 nitroalkenes by this process, not really worth at small scale.There’s a reason nitroethane is expensive besides dumb regulations
Bien sûr.100g of your alkene can be reacted scaling reagent linearlly, except maybe less ipa idk exactly I go by eye, in a 1L erlenmeyer no problem.I reckon your could push 200 but overfilling past a certain point is not kosher
I don’t know what alphastoff is but if it’s for solvent purposes xylene for sure, maybe dcm, petroleum ether, whitespirt.Providing the copy of the procedure might be helpful for other members to chime in.
Yes, it works great on my own experience.Brine wash organic layer after basification removes a lot of water, I’ve done so in a pinch when I didn’t have a drying agent on hand and it was enough for a decent yield, not too far off the sol. dried over a drying agent.Don’t overdo it and let it...
He’s worried because it’s happening before alkali addition, but if I am not wrong it can happen before, the alkali added just brings the phenomenon to completion.
No, 2 layers is what you want.As the aq. layer gets saturated with water soluble salts it pushes the dillute isopropanol-freebase sol. out of the aq. layer.This property of isopropanol, as opposed to the other primary OH-s, to separate from water when salts are dissolved is exactly why it’s used...
You answered your own question, it’s likely decomposition products of the “a-oil” reacting with air, which are impurities as people said above.Just don’t clean in any way and you get that smell, simple.If you’re looking to purify then “flavor” just don’t clean it, doing it after doesn’t make...
Some people report it’s not etno2, I don’t remember why or where I read it but I bet I can dig it up.
Either way great scheme to divert nitroethane if they’re replacing it with something else.
See for yourself, get some dry acetone (distilled or dried over a drying agent) and dissolve some of that dutch paste.See how much you’re left with and let’s start from there.
Most often amphetamine laboratories are siezed with amounts of caffeine, indicating they cut at the source.Something...