反应详情

Tert-Butylchlorodiphenylsilane (2.0 ml) was added in four portions to a solution of tert-butyl [(1R,2R)-2-hydroxy-1-(3,4,5-trifluorophenyl)propyl]carbamate (610 mg) and imidazole (817 mg) in DMF (3 ml) in a nitrogen atmosphere, and the reaction solution was stirred at room temperature for three hours. Ethyl acetate was added to the reaction solution, which was then sequentially washed with water, 1 N hydrochloric acid, water, a saturated sodium bicarbonate solution, and brine. The organic layer was dried over anhydrous magnesium sulfate, and then the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane:diethyl ether 49:1 to 19:1) to obtain 684 mg of the title compound.

1. washwas then sequentially washed with water, 1 N hydrochloric acid, water
2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
3. customthe solvent was evaporated under reduced pressure
4. customThe resulting residue was purified by silica gel column chromatography (hexane:diethyl ether 49:1 to 19:1)