Question

I need to write out a procedure for extraction and recrystallization of a 1:1 (by mass) mixture of 1,4-dichlorobenzene/ethyl 4-aminobenzoate.

So far, I have that I am starting with extraction using 1 g. of the mixture and dissolving it in about 15mL of diethyl ether. Then I am putting it in a separatory flask and adding 15mL of 1M HCl to get layers. To the organic layer, I will add sodium sulfate and put in rotovap to get a solid. To the aqueous layer I will add 6M sodium hydroxide to get the pH above 7 and use vacuum filtration to get the solid.

Here are my questions:

So far, am I using the right chemicals and concentrations?

Which layer will be the organic layer? The top?

I can't quite remember the steps/chemicals needed for recrystallization of both compounds. Can someone help me here?

The chemicals available in the lab will be the following:

1:1 mixture (by mass) of 1,4 -dichlorobenzene/ethyl 4-aminobenzoate

Sodium sulfate

Diethyl ether

Hydrochloric acid (1 M or 3 M)

Sodium hydroxide (3 M or 6 M)

TLC solvents (pre-mixed ethyl acetate/hexanes mixture)

95% ethanol

Methanol

Distilled water

Answer 1