Catalyst: Pd(dppf)Cl2 Solvent:toluene Base: tripotassium diphosphate
I keep encountering the formation of a slurry while performing solvent extraction (work-up process). I am using a trichloromethane and water extraction system. The slurry forms at the organic phase and does not separate even after addition of brine. Sonication does help, but only to a certain extent. Are there any faster methods?
I have thought of letting the slurry through and subsequently removing the water content using magnesium sulphate. However, I am afraid that this will leave the previously added NaCl as an impurity in the organic extracts after the filtration steps (to remove the hydrated magnesium phosphate, and subsequent removal of trichloromethane via vacuum distillation...
i think it may be a heating reaction so after completion of the reaction bring it to room temperature then filter through celite ,wash with a EA and not methanol or water .
Some time Chloroform and water makes slurry. Toluene ,chloroform and water makes tri-layers which is more complex. As you are using tripotassium diphosphate as a base add more water and extraced with excess of ethyl acetate, it will separete layers .
Remove the toluene by rotary evaporator first and then do the work up.
First, rotavapor the reaction mixture and then do your work up as you mentioned. In this way, you will get rid of the slurry you always encounter and also increased the yield.
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