反应详情

5.68 g (11 mmol) of the obtained alcohol form was dissolved in methylene chloride (60 mL) and 2.3 mL (16.5 mmol) of triethylamine was added thereto under a nitrogen atmosphere. 1.02 ml (13.2 mmol) of methanesulfonyl chloride was added to the mixture under ice-cooling and the mixture was stirred at room temperature for 30 minutes under a nitrogen atmosphere. Water was added to the reaction mixture and the methylene chloride layer was washed with water and a saturated NaCl solution and dried over anhydrous magnesium sulfate. After filtration, the solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (eluting solvent: hexane/ethyl acetate=3/2) to obtain 6.09 g (yield: 93%) of the title compound.

1. temperaturecooling
2. washthe methylene chloride layer was washed with water
3. dry with materiala saturated NaCl solution and dried over anhydrous magnesium sulfate
4. filtrationAfter filtration
5. distillationthe solvent was distilled off under reduced pressure
6. customthe residue was purified by silica gel column chromatography (eluting solvent: hexane/ethyl acetate=3/2)