HRID735174

反应详情

EQUATION

反应方程式

HRID 735174 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A reaction mixture of 100 mg (0.26 mmol) of (E)-N-(4′-chlorobiphenyl-4-yl)-3-(4-chloromethylphenyl)acrylamide, 70 mg (0.77 mmol) of 2-methoxyethylmethylamine, and 140 mg (1 mmol) of potassium carbonate in 10 mL of acetone is agitated for 24 hours at reflux temperature. The reaction mixture is evaporated down. The residue is purified by column chromatography on silica gel (eluant: dichloromethane/ethanol/ammonia (20/1/0.1)). Yield: 92 mg (81% of theory); melting point: 222° C.-223° C.; C26H27ClN2O2 (M=434.96); calc.: molecular ion peak (M+H)+: 435/37(Cl); found: molecular ion peak (M+H)+: 435/37(Cl); Rf value: 0.4 (silica gel, dichloromethane/methanol/ammonia (20:1:0.1)).

WORKUP

后处理

  1. temperatureat reflux temperature
  2. customThe reaction mixture is evaporated down
  3. customThe residue is purified by column chromatography on silica gel (eluant: dichloromethane/ethanol/ammonia (20/1/0.1))