HRID1990764

反应详情

EQUATION

反应方程式

HRID 1990764 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,5-Difluoro-4-formylbenzonitrile (3.60 g, 0.0215 mol; see step (ii) above) was dissolved in 50 mL of methanol and cooled on an ice bath. Sodium borohydride (0.815 g, 0.0215 mol) was added in portions with stirring and the reaction was left for 45 min. Water (300 mL) was added and thereafter carefully 2M HCl was added until an acidic pH was attained. The mixture was extracted three times with diethyl ether, and the combined ethereal phase was washed with water, dried (Na2SO4) and evaporated. The crude product crystallised soon and could be used without further purification.

WORKUP

后处理

  1. temperaturecooled on an ice bath
  2. extractionThe mixture was extracted three times with diethyl ether
  3. washthe combined ethereal phase was washed with water
  4. dry with materialdried (Na2SO4)
  5. customevaporated
  6. customThe crude product crystallised soon
  7. customcould be used without further purification