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
- 0 °C
PROCEDURE
实验过程
At −10° C., 112.8 ml (112.8 mmol) of a 1 M borane/THF complex solution are added dropwise to a solution of 20.9 g (56.4 mmol) of 2-[4-(methoxycarbonyl)benzyl]-4-[4-(methoxycarbonyl)-phenyl]butanoic acid in 600 ml of THF. The reaction mixture is then warmed to 0° C. and stirred at this temperature for 4 h. After the reaction has gone to completion, saturated ammonium chloride solution is added, the reaction mixture is diluted with water and ethyl acetate, the phases are separated and the aqueous phase is re-extracted twice with ethyl acetate. The combined organic phases are dried over sodium sulfate and, after filtration, freed from the solvent under reduced pressure. This gives 20.11 g (purity 94%, 100% of theory) of a colorless solid.
WORKUP
后处理
- additionis added
- customthe phases are separated
- extractionthe aqueous phase is re-extracted twice with ethyl acetate
- dry with materialThe combined organic phases are dried over sodium sulfate
- filtrationafter filtration