I have been researching some procedures that I would like to dream up soon and, once again, just when I thought things were clear as glass, something comes up...
Once I have my ketone, I am interested in pursuing Methyl Man's Al/hg. Now, I understand the process but I have recently stumbled across some posts touting the benefits of distilling the freebase. Am I going crazy or does Methyl Man's writeup not include a distillation of the freebase? I see at the end of the procedure he calls for a recrystallization of "raw odoriferous product" but I saw a post from Rhodium that stated both freebase distillation as well as recrystallization should be done. Is recrystallization the only method Methyl Man uses to obtain a pure product? Can an A/B & a distillation be done on the xylene after it has been washed and dried?
I am very interested in getting the purest product possible...I have chosen not to skimp on chems or equipment. If anyone could help me out, that'd be greatly appreciated...
I can't remember off the top of my head if MM distills his freebase or not, but if you want the purest product possible, do a distillation. It might cost you a few hours, but it's worth it.
But I would advise you do.
The minimum is a complete A/B, read the post from MaDMAx on the newbee forum.
After the A/B then you distill to get the freebase.
This is where I feel MM has left some pieces out because in his write-up, he doesnt even do an A/B, just cleans the xylene or toluene, meaning that anything soluble in the np will stay with the freebase as impurities.
Good, that's the conclusion I have come to also...and the few hours extra for a difference you can feel in the end product sounds like a good trade to me!
So, at what point after the amination should one distill? Once the xylene is washed and dried?
First, A/B it. This will remove any unreacted MDP2P or anything that is not an amine. Then distill the freebase.
Can somebody please help me write an addendum to the MM method with a proper description of a A/B + distillation workup, and I'll add it to the document at my page.