HRID558987

反应详情

EQUATION

反应方程式

HRID 558987 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperatureThe mixture was cooled in an ice/water bath
  2. stirringthe mixture stirred for 30 min
  3. filtrationfiltered through Celite®
  4. customevaporated in vacuo
  5. filtrationbrine, filtered through Celite®
  6. customseparated
  7. customthe organic layer was dried
  8. customevaporated in vacuo
  9. customto give a white solid