HRID2231952
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe temperature maintained for several hours
- temperaturefinally increased to 90° for two hours
- customThe solvent was evaporated
- extractionextracted from alkaline water with diethyl ether
- customto remove unreacted
- extractionextracted several times with methylene chloride
- dry with materialThe methylene chloride was dried
- customevaporated