HRID354257

反应详情

EQUATION

反应方程式

HRID 354257 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

16.1 g (0.1 mol) of 2,6-dichlorotoluene and 19.8 g (0.3 mol) of potassium hydroxide (85%) are heated in 30 ml of diethylene glycol at a bath temperature of 190° C. for 18 hours. The water released by the reaction is distilled off. After cooling, the reaction mixture is stirred with 100 ml of water until a solution is obtained and extracted three times with 50 ml of dichloromethane. The aqueous phase is admixed with 35 ml of 30% hydrochloric acid and extracted three times with 70 ml of dichloromethane. The organic phases are dried over sodium sulphate and concentrated under reduced pressure. 3-Chloro-2-methylphenol is obtained as a solid (12.4 g, content by HPLC: 83%, 72% of theory).

WORKUP

后处理

  1. distillationis distilled off
  2. temperatureAfter cooling
  3. customis obtained
  4. extractionextracted three times with 50 ml of dichloromethane
  5. extractionextracted three times with 70 ml of dichloromethane
  6. dry with materialThe organic phases are dried over sodium sulphate
  7. concentrationconcentrated under reduced pressure