HRID1048265
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
To a solution of 3 g (6.9 mmol) of (S)-ethyl 242S,3R)-3-(3-chlorophenyl)-2-(4-chlorophenyl)-6-oxopiperidin-1-yl)butanoate (Example 9, Step A) in 45 mL of Et2O was added lithium tetrahydroborate (0.334 g, 13.81 mmol) at 0° C. After being stirred at 0° C. for 50 min, the reaction was quenched (ice cold 10% citric acid) and extracted (2×EtOAc). The combined organic layers were washed with water and sat. aq. NaCl solution, dried over MgSO4, filtered and the filtrate was concentrated under reduced pressure. Purification by flash chromatography on silica gel (eluent: 30% to 60% EtOAc/Hexanes, gradient elution) provided the title compound.
WORKUP
后处理
- customthe reaction was quenched (ice cold 10% citric acid)
- extractionextracted (2×EtOAc)
- washThe combined organic layers were washed with water and sat. aq. NaCl solution
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationthe filtrate was concentrated under reduced pressure
- customPurification by flash chromatography on silica gel (eluent: 30% to 60% EtOAc/Hexanes, gradient elution)