HRID639523

反应详情

EQUATION

反应方程式

HRID 639523 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of 4-bromomethyl-1-chloro-2-trifluoromethyl-benzene (3.94 g, 14.4 mmol) and sodium cyanide (1.06 g, 21.6 mmol) in dimethyl sulfoxide (12 mL) was heated at 50° C. for one hour. The reaction mixture was then poured on ice water and extracted four times with dichloromethane. The combined organic phases were washed with water, dried over magnesium sulfate, filtered and concentrated, leading to (4-chloro-3-trifluoromethyl-phenyl)-acetonitrile (3.19 g, 14.4 mmol) as a dark red oil. This crude material was transformed into the title compound in accordance with the general method of example H2. White solid, MS (ISP) 224.1 (M−Cl)+.

WORKUP

后处理

  1. additionThe reaction mixture was then poured on ice water
  2. extractionextracted four times with dichloromethane
  3. washThe combined organic phases were washed with water
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated