反应详情

POCl3 was added to DMF at 0-10° C. after which 50 ml of CCl4 was added at room temperature. A solution of 4.5 g (24 mmol) 1a in 50 ml of CCl4 was added slowly to the reaction mixture at about 10° C. during 1 hour. The reaction mixture was refluxed for 15 min. and a solution of 50 g of NaOAc, 3H2O in 50 ml of H2O was added and refluxing was continued for 15 min. The mixture was cooled, extracted with ether and dried over Na2SO4. 8.0 g (65%) of 2a was isolated by column chromatography using EtOAc:petroleum ether as eluent.

1. additionwas added at room temperature
2. temperatureThe reaction mixture was refluxed for 15 min.
3. temperaturerefluxing
4. temperatureThe mixture was cooled
5. extractionextracted with ether
6. dry with materialdried over Na2SO4