HRID735181

反应详情

EQUATION

反应方程式

HRID 735181 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 200 mg (0.523 mmol) of (E)-N-(4′-chlorobiphenyl-4-yl)-3-(4-chloromethylphenyl)acrylamide, 295 mg (1.56 mmol) of cyclopentylmethylamine oxalic acid acetate and 0.44 mL (3.12 mmol) of triethylamine in 5 mL of THF is refluxed for 18 hours. Then the reaction mixture is poured onto water and the precipitate formed is suction filtered. Further purification is carried out by column chromatography on silica gel (eluant: dichloromethane/methanol (10:1)). Yield: 10 mg (4% of theory); C28H29ClN2O (M=445.0); melting point: 209° C.-210° C.; calc.: molecular ion peak (M+H)+: 445/447 (Cl); found: molecular ion peak (M+H)+: 445/447 (Cl).

WORKUP

后处理

  1. temperatureis refluxed for 18 hours
  2. additionThen the reaction mixture is poured onto water
  3. customthe precipitate formed
  4. filtrationfiltered
  5. customFurther purification