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.