Author Topic: Problem forming the oxime  (Read 3266 times)

0 Members and 1 Guest are viewing this topic.

hypo

  • Guest
no acid needed.
« Reply #20 on: August 15, 2004, 04:46:00 PM »
you only need acid if you don't reflux. add a few ml of water instead.


angryscientist

  • Guest
reduction deception
« Reply #21 on: August 17, 2004, 03:38:00 AM »
Friends,

My friend got his first trials done with his oxime.

But first he would like to tell everyone (pots) that his oxime always oils out too, but in the freezer, for 2 days it all crystallizes. Problem: takes more than a week to dry under high vacuum. Anyone can help out with this?

Now, after tiring hours of drying, he decided to recuce his oxime like he read somewhere, using sodium metal.
He is an impatient fellow and proceeded w/ 2x the original description, so 10 g sodium should be added, but instead of 10g sodium, he put 1 extra gram; "no big deal", he thought, those sodium pieces stink cause of the hexane and are a pain in the balls to cut into small pieces. He heated to reflux, added sodium slowly and the reflux continued from reaction, everything looked beautiful - until he added 32g H2SO4 in 400 ml water. Well, in a first moment, the solution crystallyzed abruptly with a sudden exothermic reaction. He waited until everything went into solution and repeated the addition, and it happened again but not violently. He continued adding and finally the clog didnt form anymore; everything seemed normal. he went on with the EtOH removal under vacuum and DCM (2x60ml) washes, threw DCM away. When he finished the DCM washes, he measured PH so he could basify and extract, but the solution was VERY basic!!! Shit ( he thought) what went wrong??? might it be that darn extra gram of sodium? PH was over 14.  Did he loose his (hopeful) MDA freebase or is it still in solution? Was it or was it not the extra gram of sodium? what else could it be??

he will, in the future, try the al/Hg reduction in Acetic. for cost reduction purposes, but he wants to get through with this one first.

madprosr

  • Guest
seeding the oxime
« Reply #22 on: August 17, 2004, 08:40:00 AM »
swim pretended his first batch of this oxime once, it appeared in thin crystals after cooling overnight but he made the mistake of trying to rinse the slush in his buchner filter and it went right through the paper. further cooling didn't help so it was decanted and spent more than a week being smeared on a plate and chopped alternately. antibody's AcOH/Al/Hg worked as expected. better in EtOH than MeOH (many emulsions when extracting with toluene in the later case).

once he got a seed crystal it helped alot in crystallizing waxy, chunky oxime which would stick to the bottom of the beaker. mda.hcl from this route also looked different than the mdma he had seen, flakier, less granular, and spectacularly white. he did find it a good idea to distill the ketone twice (post-performic) if doing simple distillation... but a nice vigreaux column does a better job with less loss in one run. a real column is the best 30 bux you ever spend.

now dream us some mda. don't cook and sell at the same time. first one, then stash, then the other. the most likely person to get you busted is your (ex)girlfriend.

and somebody nice test Half-a-Pints NH2OH synth on our 'tone!

angryscientist

  • Guest
Reducing surprises
« Reply #23 on: August 19, 2004, 06:32:00 PM »
My friend continued his quest to reduce precious oxime. He proceeded as sonson instructed and evaporated etoh again. Now he tested ph before washing w/ DCM. Washed, basified w/ approx. 60g 25% naoh and as the solution heated up w/ basification, he decided to put it in the freezer and cool it down before shaking w/ DCM, cause shaking warm dcm brough to him bad memories.

when he came back from lunch, stuff had crystallized...

he separated it from the water and tried to dillute it in DCM - not so much success. it did go in but not completely.
he also dilluted a small part of these crystals in IPA and added hcl in water, and ether. He is not sure stuff completely dilluted and crystllized but some white nebulous solution showed up and he filtered it.
anyone here know exactly what happened?