反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 40 °C
PROCEDURE
实验过程
351 mg (9.28 mmol) of sodium borohydride were added to 2.17 g (8.44 mmol) of the compound from Example 129A in 38 ml of ethanol and 16 ml of ethyl acetate under argon, and the mixture was stirred at 40° C. for 1 h. The reaction mixture was added to saturated aqueous ammonium chloride solution and ethyl acetate, the phases were separated, the aqueous phase was extracted twice with ethyl acetate, and the combined organic phases were dried over magnesium sulfate, filtered and concentrated. The crude product was purified by flash chromatography on silica gel (mobile phase: toluene/ethyl acetate 9/1) to result in 1.59 g (73% of theory) of a mixture of the diastereomers of the title compound.
WORKUP
后处理
- customthe phases were separated
- extractionthe aqueous phase was extracted twice with ethyl acetate
- dry with materialthe combined organic phases were dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
- customThe crude product was purified by flash chromatography on silica gel (mobile phase: toluene/ethyl acetate 9/1)