反应详情

5.68 g (11 mmol) of the resulting alcohol derivative were dissolved in methylene chloride (60 ml) followed by the addition of 2.3 ml (16.5 mmol) of triethylamine under a nitrogen atmosphere, the addition of 1.02 ml (13.2 mmol) of methanesulfonyl chloride with ice-cooling, and stirring for 30 minutes at room temperature under a nitrogen atmosphere. Water was then added to the reaction solution followed by washing the methylene chloride layer with water and a saturated aqueous solution of sodium chloride and drying with anhydrous magnesium sulfate. After filtering, the solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=3/2) to obtain 6.09 g of the desired compound (93%).

1. temperaturecooling
2. washby washing the methylene chloride layer with water
3. dry with materiala saturated aqueous solution of sodium chloride and drying with anhydrous magnesium sulfate
4. filtrationAfter filtering
5. distillationthe solvent was distilled off under reduced pressure
6. customthe residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=3/2)