HRID602990

反应详情

EQUATION

反应方程式

HRID 602990 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the mixture of 42 mg (0.08 mmol) of ethyl 3-(1-{1-[(4-chlorophenyl)(3-cyanophenyl)methyl]azetidin-3-yl}-2-fluoro-2-methylpropyl)-5-fluorobenzoate in 3 mL of THF was added 0.18 mL (0.36 mmol) of 2 M LiBH4 solution in THF and the solution was stirred overnight at rt. Then it was poured into 20 mL of CH2Cl2 and 5 mL of water. The water layer was extracted with CH2Cl2 and the combined organic layer was concentrated. The residue was purified by silica gel chromatography with hexane/ethyl acetate to afford the title compound as a white solid; Mass Spectrum: m/e=481 (M+1, 35Cl), 483 (M+1, 37Cl).

WORKUP

后处理

  1. extractionThe water layer was extracted with CH2Cl2
  2. concentrationthe combined organic layer was concentrated
  3. customThe residue was purified by silica gel chromatography with hexane/ethyl acetate