HRID491003

反应详情

EQUATION

反应方程式

HRID 491003 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

5.00 g (0.027 mol) of 2-chloro-6-ethylbenzoic acid in 120 ml of chlorobenzene are introduced into a reaction vessel and heated to 90° C. 0.1 g of α,α′-azoisobutyronitrile is then added, followed by 5.04 g (0.03154 mol) of bromine in 25 ml of chlorobenzene, which is metered in the course of 10 minutes. The reaction mixture is then stirred for 1 hour at 90° C. to complete the reaction. After the reaction mixture has cooled to 20° C., it is washed with 50 ml of sodium thiosulfate solution (0.1 mol), the organic phase is dried over sodium sulfate and the solvent evaporated off under reduced pressure using a rotary evaporator. The desired target compound is obtained in a yield of 6.1 g and a purity of about 74% (corresponding to 90% of theory).

WORKUP

后处理

  1. customis metered in the course of 10 minutes
  2. customthe reaction
  3. temperatureAfter the reaction mixture has cooled to 20° C.
  4. dry with materialthe organic phase is dried over sodium sulfate
  5. customthe solvent evaporated off under reduced pressure
  6. customa rotary evaporator
  7. customThe desired target compound is obtained in a yield of 6.1 g