反应详情

To a solution of 6.2 g of 2-(2,6-dichloroanilino)-phenylglyoxylic acid in 30 ml of dimethylformamide were added 3.3 g of anhydrous sodium acetate and then dropwise added 3 ml of ethyl bromide under ice-cooling. The mixture was stirred at room temperature for 10 hours. Thereafter, the reaction mixture was poured into 300 ml of water and the whole mixture was extracted with benzene. The benzene extract was washed with water, dried over anhydrous sodium sulfate and then concentrated. The residue was subjected to column chromatography with silica gel (Wacogel C 200), using etherhexane (1:2) as a developing solvent, to give 5.3 g of ethyl 2-(2,6-dichloroanilino)phenylglyoxylate as yellow crystals. m.p. 84°-85° C. Yield: 78% of theoretical amount

1. extractionthe whole mixture was extracted with benzene
2. extractionThe benzene extract
3. washwas washed with water
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated