HRID260549
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
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
- additionwas added at ambient temperature
- temperaturewhile cooling in an ice bath
- extractionExtraction
- washthe organic phases .were washed
- customdried
- customThe solvent was evaporated under reduced pressure
- customto obtain 180 mg of crude product which
- customwas crystallized from ethyl acetate