HRID1592330

反应详情

EQUATION

反应方程式

HRID 1592330 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of N-cyclopropyl-3-(4-fluorophenyl)propionamide (4.3 g, 20.8 mmoles) in 30 mL of dry tetrahydrofuran at 0° C. was added 1 equivalent of lithium aluminumhydride in tetrahydrofuran dropwise, and the mixture was refluxed for 2 hours. After cooling to room temperature was added sodium sulfate decahydrate slowly and the mixture was stirred for 0.5 hours. It was filtered through a plug of Celite® and evaporated to give an oily residue. It was purified by clolumn chromatography on silica gel with elution by 6:94 methanol-methylene chloride followed by 0.6:5.4:94 cNH4OH-methanol-methylene chloride to give 1.4 g of N-cyclopropyl-3-(4-fluorophenyl)propylamine and 1 g of N-propyl-3-(4-fluorophenyl)propylamine.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 2 hours
  2. filtrationIt was filtered through a plug of Celite®
  3. customevaporated
  4. customto give an oily residue
  5. customIt was purified by clolumn chromatography on silica gel with elution by 6:94 methanol-methylene chloride