HRID558987
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
To a solution of 4-cyano-N-(2-furan-2-ylphenyl)-3,N-dimethylbenzamide from Example 21C (198 mg, 0.626 mmol) in methanol (10 ml) was added cobalt (II) hexahydrate (300 mg, 1.25 mmol). The mixture was cooled in an ice/water bath and sodium borohydride (237 mg, 6.26 mmol) was added portionwise. The mixture was allowed to warm to room temperature and stirred for 2 h. Ammonia solution (4.0 ml) was added and the mixture stirred for 30 min, filtered through Celite® and evaporated in vacuo. The residue was taken up in chloroform and brine, filtered through Celite®, separated and the organic layer was dried and evaporated in vacuo to give a white solid; yield 200 mg, 100%.
WORKUP
后处理
- temperatureThe mixture was cooled in an ice/water bath
- stirringthe mixture stirred for 30 min
- filtrationfiltered through Celite®
- customevaporated in vacuo
- filtrationbrine, filtered through Celite®
- customseparated
- customthe organic layer was dried
- customevaporated in vacuo
- customto give a white solid