反应详情

To a solution of (2R,4R)-1-allyloxycarbonyl-2-[2-(imidazol-1-yl)ethyl]-4-hydroxypyrrolidine (9.19 g) in dichloromethane (92 ml) were dropwise added triethylamine (5.79 ml) and methanesulfonyl chloride (3.22 ml) under ice cooling with stirring, and the solution was stirred at the same temperature for 1 hour. The reaction mixture was poured into water and extracted with dichloromethane. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and evaporated in vacuo. The residue was purified by silica gel chromatography eluting with a mixture of chloroform and methanol (9:1, V/V) to give (2R,4R)-1-allyloxycarbonyl-2-[2-(imidazol-1-yl)ethyl]-4-(methanesulfonyloxy)pyrrolidine (4.24 g).

1. stirringthe solution was stirred at the same temperature for 1 hour
2. extractionextracted with dichloromethane
3. washThe organic layer was washed with brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customevaporated in vacuo
6. customThe residue was purified by silica gel chromatography
7. washeluting with a mixture of chloroform and methanol (9:1, V/V)