Cause I am in learning stage, I did a HALF BATCH MethylMan wacker as followed:
Methanol + PdCl2 prestired for 6 hours. Added labgrade 1,4-Benzoquinone and stired for 2 hours until nearly dissolved. Added tap water and dripped in SafroleĀ over 60 minutes. Let stir under reflux (80-85 C) for 8 hours. Made the acidwater as read in MM recipe. Dripped filtered (nearly nothing in filter, except PdCl2) post-wacker solution into acidwater, oil fell out to the bottom. Collected the oil (about 100ml), washed waterlayer with 100ml, 50ml, 50ml DCM to get the rest out of it. Combined oil and DCM washes. Put in freezer overnight. Next day the solution was frozen, but turned back into liquid after a few seconds in handwarm waterbath (this should not happen, why was it frozen?). Did the Bicarb and the NaOH washes, excluded NaCl wash, cause i had only jodized tablesalt. Distilled the 300ml oil/DCM. First without vacuum the DCM was coming off at 40 C, then another liquid under vacuum came over (25 C on my distilling thermometer ), about 50ml. Changed flask and continued distillation. No Safrole came over, but when Ketone temp was reached, just about 20g yellowish MDP2P was collected. Temp decreased, but there was still about 200ml left in the distilling flask. Stopped distilling, but the dark liquid turned immediatly into stonehard black tar, which was very hard to remove. What was wrong ? Anyone an idea ? Thanx and greetingsā¦
please help me