HRID1458749

反应详情

EQUATION

反应方程式

HRID 1458749 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 4-[2-(4-morpholinyl)ethoxy]benzonitrile (0.93 g, 4 mmol), ethanol (100 ml), CHCl3 (4 ml) and PtO2 (100 mg) is hydrogenated at 45 psi on a Parr hydrogenator for 8 hours. Concentrated HCl (2-3 drops) is then added to the reaction mixture, and the hydrogenation is continued for another 10 hours. The catalyst is removed by filtration, the filter cake is washed with ethanol and then the filtrate is evaporated to dryness. The residue is dissolved in water and then is saturated with solid K2CO3. The mixture is extracted with CH2Cl2 and then the CH2Cl2 layer is dried over K2CO3 and evaporated to afford 0.75 g (79%) of 4-[2-(4-morpholinyl)ethoxy]phenylmethylamine.

WORKUP

后处理

  1. waitthe hydrogenation is continued for another 10 hours
  2. customThe catalyst is removed by filtration
  3. washthe filter cake is washed with ethanol
  4. customthe filtrate is evaporated to dryness
  5. dissolutionThe residue is dissolved in water
  6. extractionThe mixture is extracted with CH2Cl2
  7. dry with materialthe CH2Cl2 layer is dried over K2CO3
  8. customevaporated