DMF Distillation

The Protocol of DMF Distillation

1. First add DMF (from the carboy) to the filteration flask(2L),and then add two spoons of Calcium Hydride.

2. Stir DMF for around 4hours (with vigorous stirring) or over night. (To get rid of water)

3. Stop the stirring and let DMF bottle stand for a while. And then filter DMF to remove the base. (The calcium hydride can be reused for next time, you could add crude DMF into the flask directly)

4. Add the filtrated DMF into the big RBF of distillation apparatus inside the solvent room. Turn on the circulation water, heating mantle and the pump.

5. Reflux DMF for 1h without collecting (remove the amine) After that start collecting the DMF.

Attention:

a. In the first step, we can’t change the sequence of adding DMF fisrt and then Calcium Hydride,which will absorb the water in the air.