01-03-04 01:25
No 480216
I have finished the BS Wacker 2 hours ago. Used N,N-Dimethylformamide 300ml, 2g PdCl2, 160g 1,4-Benzoquinone, 50ml H2O, 130g Safrole. After 8 hours i flooded with 50ml muriatic acid in 1.5l H2O in a 4 l beaker. Why am i unable to separate the oil, which should be on bottom of the beaker. There is a lot of crap on bottom of the beaker, which i have filtered out now, but the solution is still almost black. It's looking like ../rhodium/clandestine/nasa/
(Stranger)
01-03-04 22:43
No 480297
SWIM used to have the same problem. Try flooding the reaction with a slightly higher acid water. More like 250ml to 300ml of HCI. Look real close their will be a separation. You may have to turn off the lights and shine a bright flash light in to the mix to see the separation but it is their. Also, note MM write up. He does not separate before the DCM washes. Good luck.
(Hive Addict)
01-03-04 22:56
No 480300
Your only real problem i think is that the BS benzo wacker has the problem of the water layer and organic layer have just about the same color. So you have to just look really hard for the separation. Sometimes you even have to use a flashlight, just like Just4Fun said.
It is seductive, way too seductive. -Eleusis