cooked (too hot) MM wacker !!!

[methlab]

Hi! I think i ran the MM wacker too hot. Instead of a mild reflux, i did it around 80-85 degrees Celsius. Methanol was flowing from the condenser (as i read in Al/Hg). Could this be the reason for my reduced yield ? Have heard that MDP2P is converted into Iso-something, when run too hot. Got only  about 20g MDP-2-P from 89g Safrole (half batch MM wacker, cause i am still learning and didn't want to fuck up this expensive stuff). What was wrong ?

[Vibrating_Lights]

The hotter you run it the better just keep it all inside the flask.  It is good too to start the drip whit it already refluxing.  amalgamate the al with reflux then turn off the heat as you start the drip..  This will prevent too much going too fast.  As you do it more it will get interactive.  when you start with it already hot it is pretty responsive.  Low yeilds usually result from basifying too fast or impure ketone. NaOH will hydrolize the amine if it gets too hot during the basification. It'll take that NH2 and turn it into a OH.  IF you distill your freebase you can recover any alcohol and then turn it back into ketone it a MnO2 microwave.  Those reactions are awesome.
As above so is below

[Rhodium]

IF you distill your freebase you can recover any alcohol

Obviously an acid/base extraction is performed after the amination making the alcohol ends up in the non-polar wash of the acidified aqueous solution containing the MDMA hydrochloride.

Post 481437

(Rhodium: "How to isolate the byproduct MDP2Pol for re-use", Novel Discourse)