Extraction into organic solvent: Using a plastic pipette transfer the solution from the
filter flask into a centrifuge tube. Add one ml of saturated sodium chloride. Extract the
solution with 3 ml methylene chloride (don’t forget to release the pressure by removing
the cap after shaking). If an emulsion is formed, it can be broken by centrifuging the
solution for 2 minutes. Transfer the organic layer into a clean centrifuge tube. (In some
cases a third layer is observed between the organic and aqueous phases. In this case
transfer only the bottom clear methylene chloride layer. Repeat the extraction two more
times with fresh portions of 3 ml methylene chloride and combine the organic layers.
Wash the combined organic fractions with 1 ml saturated sodium chloride solution and
separate the organic layer. Dry the organic layer by adding anhydrous sodium sulfate.
Remove the dry organic layer into a pre weighed 50 ml filter flask. Wash the drying
agent twice with 1 ml methylene chloride and add it to the filter flask. Evaporate the
methylene chloride using a sand bath (in the hood !). Make sure that the temperature of
the sand is not higher then 80o
C! Weigh the dry flask to find the “crude” product weight.
Keep a sample for melting point.