HRID2165155

反应详情

EQUATION

反应方程式

HRID 2165155 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

9.3 g (49 mmol) of crude 2-(6-methoxyindan-1-yl)acetonitrile are dissolved in 100 ml of methanol and, after the addition of 1 g of Raney nickel and 20 g of liquid ammonia, are hydrogenated at 70°-80° and 120 bar pressure. After 3 hours, the catalyst is filtered off from the methanolic solution and is subsequently washed with methanol. The methanolic solutions are combined and rendered acidic with hydrochloric acid. The acidic solution is concentrated to dryness by evaporation in vacuo, and the residue is dissolved in 100 ml of water, rendered alkaline with concentrated sodium hydroxide solution and extracted by shaking with diethyl ether. The ethereal phases are washed with saturated sodium chloride solution and dried over magnesium sulphate. After removing the solvent, crude 2-(6-methoxyindan-1-yl)ethylamine is obtained in the form of a yellow oil.

WORKUP

后处理

  1. customare hydrogenated at 70°-80°
  2. filtrationthe catalyst is filtered off from the methanolic solution
  3. washis subsequently washed with methanol
  4. concentrationThe acidic solution is concentrated to dryness by evaporation in vacuo
  5. dissolutionthe residue is dissolved in 100 ml of water
  6. extractionextracted
  7. washThe ethereal phases are washed with saturated sodium chloride solution
  8. dry with materialdried over magnesium sulphate
  9. customAfter removing the solvent