HRID986258

反应详情

EQUATION

反应方程式

HRID 986258 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 1.44 g of sodium hydride in 100 ml of dimethylformamide is treated within 10 minutes with 9.75 g of 9-acridanone and held at 50° for 2 hours. At 120° there are then added 9.5 g of 4,4-diethoxybutyl chloride. After 16 hours, the mixture is cooled, poured into water and extracted with dichloromethane. The extract is dried over sodium sulfate and evaporated. The residue is extracted with hexane and crystallized twice from hexane. There is obtained 10-(4,4-diethoxybutyl)-9-acridanone of metling point 73°-74.5°.

WORKUP

后处理

  1. waitAfter 16 hours
  2. temperaturethe mixture is cooled
  3. extractionextracted with dichloromethane
  4. dry with materialThe extract is dried over sodium sulfate
  5. customevaporated
  6. extractionThe residue is extracted with hexane
  7. customcrystallized twice from hexane