the 8.1g ketone distilled from 90-106C was dripped into a directly-scaled Osmium MeNH2/al/hg utilizing small square MeNH2 crystals extracted from nh4cl with IPA, crystalized, then dcm-washed. swim used 4g Al, 9g MeNH2.hcl freebased with NaOH solution before addition. solution was homogenous and at pH 9 (bit of extra NaOH) after 6 hours, basified to pH 12, extracted 3x 50ml toluene. washed 3x 50ml brine, dried over 7g MgSO4.1h2o, and gassed 3.6g mdma.hcl
after the ketone was distilled, 8.9g of slightly sticky when cold yellowish oil was collected peaking at 114C.
the rest of his 65g batch of iso turned into super-sticky brown sludge. eww...
swim is thinking it has to be insufficient stirring. his 75% m/m performic was done on an IKA Labortechnik hotplate/stirrer which no longer heats. the last three bad performics were hydrolized with a Marec Thermodyne 3.
to the glycol from 65g iso in a 500ml rb flask, swim added 360g 15% h2so4, and stirred with the Marec on max with a 1/2" octagonal stir bar, creating a vortex 3/4" across and perhaps 1" deep.
it was held at 60C for 6h, until swim realized that the orange color was never going away completely, turning a sweet red-brown, it was just going to stay orange as it burned.
any advise on this hydrolysis would be enormously appreciated.
how can swim have glycol contamination after such an excessive hydrolysis?
swim is going to try an oxone epoxidation followed by hydrolizing on the IKA stirrer, pulling the waterbath out occasionally to heat it up.
that or he could try to rig a mechanical stirrer for hydrolysis, he has a small AC motor rated at 2000 rpm, is this about right? where to find a sheet of teflon?
"one way or another, sooner or later, this darkness has got to give" -the dead