HRID2231952

反应详情

EQUATION

反应方程式

HRID 2231952 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

11.3 g (72.8 mmol) 4-chloro-2,3,5-trimethylpyridine was dissolved in 50 ml acetic acid and heated to 60° C. and 6.2 ml (50% H2O2) was added slowly and the temperature maintained for several hours and finally increased to 90° for two hours. The solvent was evaporated and extracted from alkaline water with diethyl ether to remove unreacted starting material. The water phase was saturated with sodium chloride and extracted several times with methylene chloride. The methylene chloride was dried and evaporated to give 10.1 g of product. Yield 83%. M.p. 147°-148° C.

WORKUP

后处理

  1. temperaturethe temperature maintained for several hours
  2. temperaturefinally increased to 90° for two hours
  3. customThe solvent was evaporated
  4. extractionextracted from alkaline water with diethyl ether
  5. customto remove unreacted
  6. extractionextracted several times with methylene chloride
  7. dry with materialThe methylene chloride was dried
  8. customevaporated