反应详情

温度

120 °C

1-Bromo-3-(trifluoromethylthio)-prop-2-ene (1.05 g, Example B) is added to a mixture of 1A (1.08 g), sodium hydride (60% in oil, 0.18 g) and N-methylpyrrolidone (20 ml) and DMF (1 ml). The reaction mixture is stirred for 6 hours at 120° C. The remaining sodium hydride is deactivated and the resulting mixture is diluted with pentane/ethyl acetate (by volume ration 1/1) and filtered through a bed of silica gel. The filtrate is washed with water. The organic layer is dried with anhydrous magnesium sulfate, filtered and evaporated in vacuo. Purification by flash chromatography (silica gel: pentane/ethyl acetate 10/1 v/v) yields 0.3 g of the title compound.

1. filtrationfiltered through a bed of silica gel
2. washThe filtrate is washed with water
3. dry with materialThe organic layer is dried with anhydrous magnesium sulfate
4. filtrationfiltered
5. customevaporated in vacuo
6. customPurification by flash chromatography (silica gel: pentane/ethyl acetate 10/1 v/v)