反应详情

1.5 g of the compound obtained in Example 2 was dissolved in 40 mL of dichloromethane, and the resulting solution was cooled to below 5° C. To the solution, 3.6 g of p-toluenesulfonyl chloride and 1.9 g of triethylamine were added dropwise, and the resulting mixture was warmed to room temperature, stirred for 6 hours and washed twice with 20 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 1.5 g (yield of 48%) of the title compound as an oil.

1. temperaturethe resulting solution was cooled to below 5° C
2. washwashed twice with 20 ml portions of water
3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure