反应详情

To a solution of (2S,4R)-4-(tert-butyldimethylsilyloxy)-1-(tert-butoxycarbonyl)-2-hydroxymethylpyrrolidine (5.3 g) and methanesulfonyl chloride (1.49 ml) in dichloromethane (40 ml) was added dropwise triethylamine (3.2 ml) at 0° C. After one hour, the reaction mixture was washed in turn with 1N-hydrochloric acid, water and brine. The organic layer was dried over magnesium sulfate, and evaporated to give an oil, which was chromatographed on silica gel (250 ml) eluting with a mixture of hexane and ethyl acetate (2:1, V/V) to give (2S,4R)-4-(tert-butyldimethylsilyloxy)-1-(tert-butoxycarbonyl)-2-methanesulfonyloxymethylpyrrolidine (6.06 g).

1. washthe reaction mixture was washed in turn with 1N-hydrochloric acid, water and brine
2. dry with materialThe organic layer was dried over magnesium sulfate
3. customevaporated
4. customto give an oil, which
5. customwas chromatographed on silica gel (250 ml)
6. washeluting with a mixture of hexane and ethyl acetate (2:1, V/V)