SWIM didn't re-distill his MDP-2-P, the for run was dumped and the rest all came over between 174-177 at 26.5" of Hg. .
SWIM has been doing some more reading and is really interested in higher purity of product, SWIM has read many posts on recrystallization and want to make sure SWIM gets it right. This is what SWIM plans to do.
1. Add 500 ml isopropanol to a 600 ml beaker and bring to boil
2. Add MDMA.HCL to 250 ml beaker, pour hot isopropanol into beaker to dissolve MDMA.HCL
3. Let cool to room temp
4. Filter
5. Wash crystals with some acetone
6. Do a second recovery by placing first wash in freezer and repeating
Has SWIM missed anything there?
Also SWIM would like to distill off the toluene/xylene before gassing and wanted to make sure SWIM doesn’t mess this up either.
So once SWIM has everything ready to gas, toluene (or xylene) can SWIM just throw the mixture into a distilling flask and distill off the toluene/xylene? SWIM sees that toluene should come over at 110 degrees, and xylene at 144/139/138 depending, how much toluene/xylene + MDMA.HCL freebase should be left in the flask for gassing? ~100ml?
Is this a safe method? SWIM plans on doing this under vacuum and will calculate what temp the toluene/xylene will come over at
SWIM was also thinking about doing an A/B extraction and moving the freebase into the DCM and the distilling of the DCM and gassing the DCM, but read a few posts that said gassing the freebase in DCM had poorer yields than gassing in the toluene.
If SWIM plans on doing 2 recrystallization would you still recommend doing an A/B extraction before gassing?
All suggestions welcome.
Thanks.