反应详情

温度

0 °C

A mixture of 3.0 g of 8-chloro-5-(4-chlorophenyl)-5H-indeno[1,2-d]pyrimidin-5-ol in 50 ml of methylene chloride was cooled to 0° C. under a nitrogen atmosphere. Approximately 2.7 g of diethylaminosulfur trifluoride were added and the reaction was stirred overnight. The mixture was poured into an iced solution of potassium bicarbonate and extracted with ethyl acetate. The organic extract was washed with a sodium bicarbonate solution and a sodium chloride solution, dried over magnesium sulfate, and concentrated in vacuo. Crystallization from ethyl acetate/isooctane provided 2.29 g of the desired title product, m.p. 236°-237° C.

1. extractionextracted with ethyl acetate
2. extractionThe organic extract
3. washwas washed with a sodium bicarbonate solution
4. dry with materiala sodium chloride solution, dried over magnesium sulfate
5. concentrationconcentrated in vacuo
6. customCrystallization from ethyl acetate/isooctane