反应详情

温度

-3 °C

3.0 g of the compound obtained in Example 2 was dissolved in 57 mL of dichloromethane, and the resulting solution was cooled to −3° C. To the solution, 6.1 g of diisopropylethylamine and 3.1 g of sulfuryl chloride were added, and the resulting mixture was stirred for 30 min at the same temperature and for an hour at room temperature. 20 mL of dichloromethane was added to the reaction solution, and the resulting mixture was washed twice with 40 mL portions of water. The organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was subjected to a silica gel column chromatography (eluent, n-hexane:ethyl acetate=10:1) to obtain 1.0 g (yield of 27%) of the title compound as a colorless oil.

1. washthe resulting mixture was washed twice with 40 mL portions of water
2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
3. concentrationconcentrated under reduced pressure