complete mm al/hg failure, puzzled

[homeslice]

I read on this website, forgot the name, of this guy who was performing a standard mm al/hg and it his failure went like this.

First he used different ketone as his last couple successes. This time his tone has a less flourescent yellow green and is more pickle juice colored. Smelled the same he said and tasted the same.

Amalgum -- He used 350mg hgi2 instead of hgcl2 and prestirred it a good 30 minutes it said. When he added the ingredients to the sep funnel he did so very carefully and slowly allowing the layers to seperate. He added nitro, then meoh, then ketone. His ketone sank to the bottom of the layers, he thought it floated on the other 2 layers the last couple times but he could be mistaken. The amalgum went great. Addition in 25 mins, nice and hot, blue, 1/2 up the condenser pourin like a faucet. Everything looked the same as last time except, there was much more tinfoil left. Now he didnt mean there were chunks but alot of tiny little flecks. Much more than previous attempts. His NaOH solution ate all of it though. But he trudged on, assuming it would only hurt his yields a little bit, IF he was even wrong.

Washes -- Extractions went fine with toluoene it said. During the first water wash, there was a white semi solid interface, very cruddy looking. He didnt keep it. During the 2nd there was the same but not as big. 3rd wash - normal. 4th wash he washed with saturated nacl and it went fine he said. And with a final wash he washed with dh2o again and it was fine looking. Dried with 40 grams oven dried epsoms. What are the water washes used to wash out?

Gassing -- Set up was h2so4 over anhydrous nacl saturated with muriatic. Gas traveled through a vigreux column jammed pack with cacl2. Same set up as before. Started gassing slowly and it was going fine, he could see cloudiness in the water. Stopped for a second, resubmerged and noticed a little suckback occurincg slowly. So he turned on the funnel and accidently allowed a stream of h2so4 to fall. Enough that it made the sep funnel make a glug. He reached to take the glass tube outta the solution but it was already bubbling viciously. He noticed the solution turn a little tannish with not precipitants and said mother fucker god dammed fuckin funnel thingy mother fuckin bitch. So he MAY have overgassed. Not sure. He gassed a little more but nothing. Just turned a little more tan. Obviously he saved the contents of his tan solution.

He thinks he should have at least gotten SOMETHING. After the NaOH addition it had that fishy smell that it always has in the past, signifying to him that it was a successful reaction, he said. He said he was going to look up overgassing.

Edit: Ya know even if the ketone wasnt the absolute best, it had enough qualitys to produce at least some honey... bah.. thinking too much about this is hurtin my brain

[homeslice]

[baalchemist]

A fishy smell does'nt necessarily mean success. It could simply also mean that only the nitro was reduced to methylamine. That fishy smell describes many chem scenario's, but as a definitive aroma regarding this reactions success probability it is definately not at all viable for that purpose. TLC has those answers......

[Bandil]

Sounds like you have used not-so-pure ketone, which will result in not-so-pure MDMA extracts. You only performed a simple extraction followed by a water wash. This is not enough to give a clean toluene/MDMA phase. If the ketone is clean and the reaction otherwise runs without problems you are usually able to gas and recover the product.

However, by using impure ketone and skipping a proper A/B extraction + vac. distillation, the final toluene/MDMA phase is most likely to impure to induce crystallization (oiling out instead). This is a very common problem when using the popular "quick'n'dirty" MDMA synthesis you have performed.

Basify your toluene phase and separate the water. Dry the toluene (azeotropical distillation rocks for this) and strip the toluene under some vacuum. Then distill your MDMA properly. No matter what your yields were (not if it was zero of course   ), this will give you a product which is very easy to crystallize.

It can't be said enough (heavens knows it took my alter ego ages to learn it):
Doing reactions quick'n'dirty is like pissing in your pants on a winter day - it feels nice the first few minutes... But you will regret it in the end.

Have a nice weekend!

Regards
Bandil

[homeslice]

Ive read a couple of posts calling for a vac distill before gassing but ive also read posts saying its way unnecessary. I think alot of posts by Rhodium recommended it and baalchemist said it was unnecessary. Im confused since both ways seem to work.

[Rhodium]

It depends on how you define "work". One of the ways will invariably produce nice, white crystals with little impurities, the other may or may not fail to crystallize, will most often produce off-white crystals or worse, and will always contain dimeric amine byproducts and other impurities.

Which one would you rather be offered?

[wyndowlicker]

Hey now,


Those are the last places you want to bee cutting corners.I see several possible problems.Your gas probably wast dry enough either.The tone needs to be redistilled to check its BP and in the end purity.Of course an A/B like stated above.Make it clean,clean man.Theres no other way to do your fellow man. distill your freebase from the toluene then theres no confusion.