Luke Raffanti

A Separation and Purification Scheme: Procedure

Dissolve the solid in methylene chloride: Add 2.0 mL methylene chloride to the solid in a
centrifuge tube. Carefully mix by inverting, rocking it at a rate of about of one inversion/second,
taking care not to form an emulsion.

Add 1M HCl: Add 2 mL of 1 M HCl, shake for 30 seconds, and let the layers separate. Remove
the bottom layer (the organic layer) and place it into another tube. Label the original tube “1st
HCl extraction.” Repeat with two more additions of 2 mL HCl to the organic layer, labeling each
extraction in a separate tube.

Dry the organic layer: remove any visible water from the organic layer. Add granular
anhydrous sodium sulfate until it doesn’t clump together but its texture resembles the snow in
a snow globe. Cap it and allow it to dry for at least 15 minutes.

Add 6M NaOH to the aqueous layer: With stirring, add 6 M NaOH dropwise until the mixture
becomes basic (test with pH paper).

Filter and dry the isolated base precipitate: filter the precipitate over a Hirsch funnel. Pre-
weigh a watch glass, then air dry on a watch glass. Heat gently on a hot plate (on a low heat
setting). Obtain the weight and melting point (should be around 110-111°C) of the isolated
methyl 4-aminobenzoate.

Remove the drying agent from the organic layer: use a clean, dry, pasteur pipette to transfer
the dried organic layer into a clean, dry conical 10mL erlenmeyer flask.

Evaporate the methylene chloride: place the organic layer into a hot water bath (50° C) until
the methylene chloride has evaporated. The two neutral compounds should now be dry and
have formed a solid crust in the tube.

Crystallization: prepare 8-9 mL of 95% ethanol in a tube that will be heated to boiling (about
78.5°C). Prepare a few mL of ice-cold ethanol in an ice bath for rinsing. Dissolve the impure
neutral compounds in the minimum possible amount of boiling solvent. Add just enough hot
solvent to cover the crystals before adding the crystals to the hot plate alongside the boiling
solvent. Once the solid has been dissolved, allow the flask to cool to room temperature,
insulated inside of a larger beaker and placed on top of something like a binder. After it has
cooled to room temperature, place into an ice bath if necessary to form more crystals. Moisten
the filter paper on a Hirsch funnel with a few drops of solvent. Dislodge crystals with a
microspatula, and swish and dump the crystals into the Hirsch funnel. Rinse with some ice-
cold solvent and let it dry in the funnel, before transferring to a pre-weighed watch glass to let
it dry more.