HRID1094162

反应详情

EQUATION

反应方程式

HRID 1094162 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Under ice-cooling, 11.5 g of sodium triacetoxyborohydride was added in small portions to a solution of 4.0 g of 3,4,5-trifluoroaniline and 3.6 ml cyclopentanone in 150 ml dichloroethane and 3.1 ml acetic acid, and, after rising to room temperature, stirred for 3.5 hours. Aqueous saturated sodium hydrogen carbonate was added thereto, followed by extraction with chloroform and subsequent drying over anhydrous sodium sulfate. After filtration, the solvent was evaporated under a reduced pressure, and the resulting residue was purified by silica gel column chromatography to obtain 5.4 g of N-cyclopentyl-3,4,5-trifluoroaniline.

WORKUP

后处理

  1. temperatureUnder ice-cooling
  2. customafter rising to room temperature
  3. extractionfollowed by extraction with chloroform
  4. dry with materialsubsequent drying over anhydrous sodium sulfate
  5. filtrationAfter filtration
  6. customthe solvent was evaporated under a reduced pressure
  7. customthe resulting residue was purified by silica gel column chromatography