反应详情

温度

30 °C

To 234 ml of dimethyl sulfoxide was added 32 g of trimethyl sulfoxonium iodide. To it, potassium tertiary butoxide (16 g) was added and stirred for 1 h at 20-40° C. The reaction mixture was cooled and to it was added a solution of the compound obtained in Example 2 in dimethyl sulfoxide (26 ml.) while maintaining the temperature between 20°-40° C. for 1.5 hr. The reaction mixture was quenched in cold water. The aqueous layer was extracted with ethyl acetate, washed with water, concentrated under reduced pressure followed by product distillation to give 19.6 g of 6-fluoro-3,4-dihydro-2-oxiranyl-2H-1-benzopyran (VII) in the form of a mixture of A and B as an oil.

1. temperatureThe reaction mixture was cooled and to it
2. temperaturewhile maintaining the temperature between 20°-40° C. for 1.5 hr
3. customThe reaction mixture was quenched in cold water
4. extractionThe aqueous layer was extracted with ethyl acetate
5. washwashed with water
6. concentrationconcentrated under reduced pressure
7. distillationfollowed by product distillation