反应详情

To a solution of 12.4 g of 2-(2,6-dichloroanilino)-phenylglyoxylic acid in 80 ml of anhydrous acetone were added 6.05 g of anhydrous potassium carbonate and then 8 ml of diethyl sulfate, and the mixture was stirred at room temperature for 1 hour. The reaction mixture was filtered and washed with anhydrous acetone. The filtrate was concentrated under 100 mmHg without heating. The residue was subjected to column chromatography with silica gel (Wacogel C 200), using ether-hexane (1:2) as a developing solvent, to give ethyl 2-(2,6-dichloroanilino)phenylglyoxylate. m.p. 84.0°-85.5° C.

1. filtrationThe reaction mixture was filtered
2. washwashed with anhydrous acetone
3. concentrationThe filtrate was concentrated under 100 mmHg
4. temperaturewithout heating