HRID260549

反应详情

EQUATION

反应方程式

HRID 260549 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

200 mg of the product of Stage C of Example 3 were dissolved in 5 ml of dimethyl ether of ethylene glycol and 1 ml of concentrated sulfuric acid was added at ambient temperature. After stirring for one hour, water was added while cooling in an ice bath. Extraction was carried out with dichloromethane and the organic phases .were washed and dried. The solvent was evaporated under reduced pressure to obtain 180 mg of crude product which was crystallized from ethyl acetate to obtain 140 mg of the expected product melting at 130°-132° C.

WORKUP

后处理

  1. additionwas added at ambient temperature
  2. temperaturewhile cooling in an ice bath
  3. extractionExtraction
  4. washthe organic phases .were washed
  5. customdried
  6. customThe solvent was evaporated under reduced pressure
  7. customto obtain 180 mg of crude product which
  8. customwas crystallized from ethyl acetate