HRID966959

反应详情

EQUATION

反应方程式

HRID 966959 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 4-chloro-2-[(3-hydroxy-1-phenylpropyl)amino]benzonitrile (2.3 g, 8 mmol) in dry tetrahydrofuran (50 ml) was treated with tert-butyldimethylsilylchloride (2.41 g, 2 eq.) and imidazole (1.09 g, 2 eq.) and stirred at room temperature for 1 h. The reaction mixture was diluted with water (200 ml) and the products extracted into diethyl ether (200 ml). The organic extract was dried over magnesium sulphate and concentrated to an oil. The crude product was purified on silica gel eluting with isohexane/diethyl ether (2:1) to afford the title compound as a colourless oil (2.3 g, 72%).

WORKUP

后处理

  1. extractionthe products extracted into diethyl ether (200 ml)
  2. extractionThe organic extract
  3. dry with materialwas dried over magnesium sulphate
  4. concentrationconcentrated to an oil
  5. customThe crude product was purified on silica gel eluting with isohexane/diethyl ether (2:1)