HRID363126

反应详情

EQUATION

反应方程式

HRID 363126 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
400 °C

PROCEDURE

实验过程

A solution of 150 g (0.974 mol) of 4-fluorophenylacetic acid an 1 mL of N,N-dimethylformamide in 500 mL of toluene at 40 ° C. was treated with 20 mL of thionyl chloride and heated to 400° C. An additional 61.2 mL of thionyl chloride was added dropwise over 1.5 hours. After the addition, the solution was heated at 50° C. for 1 hour, the solvent was removed in vacuo and the residual oil was distilled at reduced pressure (1.5 mmHg) to afford 150.4 g (89.5%) of the title compound, bp=68°-70 ° C.

WORKUP

后处理

  1. additionAfter the addition
  2. temperaturethe solution was heated at 50° C. for 1 hour
  3. customthe solvent was removed in vacuo
  4. distillationthe residual oil was distilled at reduced pressure (1.5 mmHg)