反应详情

A solution of 5,6-dichloroisatin (1.0 g, 4.65 mmol) in DMF (20 ml) was cooled in an ice-bath. Sodium hydride (5.11 mmol, 0.20 g 60% dispersion in mineral oil) was added and the mixture was stirred for 20 min. Ethyl 2-bromoacetate (0.37 ml, 5.11 mmol) was added and stirring was continued for 2 hours. The resulting mixture was poured into diluted hydrochloric acid (200 ml, 4M), heated to reflux for 2 hours, filtered, cooled and extracted with ethyl acetate. The organic extract was dried over magnesium sulphate and evaporated to dryness to leave the desired product (0.85 g, 67%).

1. stirringstirring
2. waitwas continued for 2 hours
3. temperatureheated
4. temperatureto reflux for 2 hours
5. filtrationfiltered
6. temperaturecooled
7. extractionextracted with ethyl acetate
8. extractionThe organic extract
9. dry with materialwas dried over magnesium sulphate
10. customevaporated to dryness