反应详情

Methanesulfonyl chloride (14 mL) was added to a mixture of N-[(1S,2R)-2-(3-amino-4-benzyloxyphenyl)-2-hydroxy-1-methylethyl]-2,2,2-trifluoroacetamide (62 g) and pyridine (34 mL) in ethyl acetate (558 mL) at room temperature with stirring, and the mixture was stirred at 40° C. for 1 hr. Ethyl acetate and water were added to the reaction mixture. The organic layer was separated, washed successively with 1 mol/L hydrochloric acid, water and brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was recrystallized from n-hexane/ethyl acetate to afford the title compound (42 g).

1. stirringthe mixture was stirred at 40° C. for 1 hr
2. customThe organic layer was separated
3. washwashed successively with 1 mol/L hydrochloric acid, water and brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe solvent was evaporated under reduced pressure
6. customthe residue was recrystallized from n-hexane/ethyl acetate