HRID26431

反应详情

EQUATION

反应方程式

HRID 26431 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The solution of 6.5 g of 3-(2-methoxyiminopropyl)-4-(4-methoxyphenyl)-1,5,6,7-tetrahydro-2H-azepinone in 150 ml of ethanol is hydrogenated at room temperature and atmospheric pressure in the presence of 10 g of Raney nickel until the uptake of 2 mole equivalents of hydrogen is complete. The mixture is filtered, the filtrate evaporated and the residue dissolved in 100 ml of water and 10 ml of 6 N hydrochloric acid. The acidic solution is washed with diethyl ether, filtered, basified with 30 ml of 3 N aqueous sodium hydroxide and repeatedly extracted with chloroform. The extract is dried, evaporated and the residue is purified by suspension in diethyl ether, to give the 3-(2-aminopropyl)-4-(4-methoxyphenyl)-1,5,6,7-tetrahydro-2H-azepinone melting at 131°-133°.

WORKUP

后处理

  1. customis hydrogenated at room temperature
  2. filtrationThe mixture is filtered
  3. customthe filtrate evaporated
  4. dissolutionthe residue dissolved in 100 ml of water
  5. washThe acidic solution is washed with diethyl ether
  6. filtrationfiltered
  7. extractionrepeatedly extracted with chloroform
  8. customThe extract is dried
  9. customevaporated
  10. customthe residue is purified by suspension in diethyl ether