HRID1748508

反应详情

EQUATION

反应方程式

HRID 1748508 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Palladium (II) acetate (90 mg), 2-(di-tert-butylphosphino)biphenyl (240 mg), sodium tert-butoxide (1.35 g), toluene (20 ml) and p-methoxybenzylamine (1.81 g) were added to 1-(5-bromopyridin-2-yl)cyclohexanecarbonitrile (2.5 g), and stirred at 100° C. for two hours. Water was added to the reaction solution, the resulting precipitate was filtered, the filtrate was extracted with ethyl acetate and the organic layer was concentrated. The residue was purified with silica gel chromatography (n-hexane/ethyl acetate) to give 1-{5-[(4-methoxybenzyl)amino]pyridin-2-yl}cyclohexanecarbonitrile (650 mg) as a solid.

WORKUP

后处理

  1. filtrationthe resulting precipitate was filtered
  2. extractionthe filtrate was extracted with ethyl acetate
  3. concentrationthe organic layer was concentrated
  4. customThe residue was purified with silica gel chromatography (n-hexane/ethyl acetate)