反应详情

To a solution of 4-(3-hydroxypropyloxy)-N-t-butyloxycarbonylpiperidine (3.82 g) in ethyl acetate (40 ml) were added triethylamine (4.1 ml) and methanesulfonyl chloride (1.37 ml) with stirring under ice-cooling, and the mixture was stirred at the same temperature for 1 hour. To the reaction mixture were added water (50 ml) and ethyl acetate (50 ml) with stirring. The organic layer was separated, washed twice with saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate and evaporated in vacuo. The resulting residue was chromatographed on silica gel (150 ml) eluting with a mixture of n-hexane and ethyl acetate (1:1 v/v). The fractions containing the desired compound were collected and evaporated under reduced pressure to give 4-[3-(methanesulfonyloxy)propyloxy]-N-t-butyloxycarbonylpiperidine (3.77 g).

1. temperaturecooling
2. stirringthe mixture was stirred at the same temperature for 1 hour
3. stirringwith stirring
4. customThe organic layer was separated
5. washwashed twice with saturated aqueous sodium chloride
6. dry with materialdried over anhydrous magnesium sulfate
7. customevaporated in vacuo
8. customThe resulting residue was chromatographed on silica gel (150 ml)
9. washeluting with a mixture of n-hexane and ethyl acetate (1:1 v/v)
10. additionThe fractions containing the desired compound
11. customwere collected
12. customevaporated under reduced pressure