HRID1450370

反应详情

EQUATION

反应方程式

HRID 1450370 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.5 g (30.3 mmol) of the chloride from Example 1, Step B and 6.3 g (30.3 mmol) of 4-aminomethyl-2'-cyanobiphenyl (prepared according to EP 459 136) were heated in 150 ml dry ethanol for 10 h. After removal of the solvent in vacuo yellow crystals formed. These were purified by suspension in acetone and dissolved, in ethyl acetate. The solution was washed with 10% sodium carbonate solution, the organic layer dried over sodium sulfate, and evaporated to dryness to give colorless crystals of the title compound, m.p. 230°-233° C.

WORKUP

后处理

  1. customAfter removal of the solvent in vacuo yellow crystals
  2. customformed
  3. customThese were purified by suspension in acetone
  4. dissolutiondissolved, in ethyl acetate
  5. washThe solution was washed with 10% sodium carbonate solution
  6. dry with materialthe organic layer dried over sodium sulfate
  7. customevaporated to dryness