HRID27438

反应详情

EQUATION

反应方程式

HRID 27438 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Hydrogenate 3.72 of 7-(4-nitrobenzyl)perhydroazepin-2-one in 50 mls of ethyl alcohol with platinum/hydrogen. After the absorption of hydrogen has ceased, filter off the catalyst and concentrate the filtrate. Dissolve the thus obtained 7-(4-aminobenzyl)-perhydroazepin-2-one in tetrahydrofuran. Add 680 mg of lithium aluminum hydride and boil the mixture under reflux. After cooling, treat it with ice-water and extract it with diethyl Dry the organic phase over sodium sulphate and concentrate it to obtain 2.0 g of the brown oily title compound.

WORKUP

后处理

  1. customAfter the absorption of hydrogen
  2. filtrationfilter off the catalyst
  3. concentrationconcentrate the filtrate
  4. dissolutionDissolve the thus obtained 7-(4-aminobenzyl)-perhydroazepin-2-one in tetrahydrofuran
  5. additionAdd 680 mg of lithium aluminum hydride and boil the mixture
  6. temperatureunder reflux
  7. temperatureAfter cooling
  8. additiontreat it with ice-water
  9. extractionextract it with diethyl
  10. dry with materialDry the organic phase over sodium sulphate
  11. concentrationconcentrate it