HRID544129

反应详情

EQUATION

反应方程式

HRID 544129 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

11 g of N-diphenylmethyl-ethylenediamine, 10.1 g of triethylamine and 7.0 g of 1-phenylethyl chloride are dissolved, while stirring, in 85 ml of acetonitrile and heated under reflux for 30 hours. The solution is concentrated by evaporation under reduced pressure, 50 ml of 10% sodium hydroxide solution are added and the mixture is extracted thoroughly by shaking with diethyl ether. The ether extracts are combined, dried over sodium sulphate and concentrated by evaporation. N-diphenylmethyl-N'-(1-phenylethyl)-ethylenediamine is obtained in the form of a yellow oil which can be purified chromatographically over silica gel with methanol/ethyl acetate (1:1) as the eluant and, for characterisation, can be converted into the dihydrochloride, having a melting point of 160° C., as described in Example 4.

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux for 30 hours
  3. concentrationThe solution is concentrated by evaporation under reduced pressure, 50 ml of 10% sodium hydroxide solution
  4. additionare added
  5. extractionthe mixture is extracted thoroughly
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated by evaporation