HRID1247947

反应详情

EQUATION

反应方程式

HRID 1247947 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.02 mole of 3-chloro-3-(3-pyridinyl)-2-propenal and 0.02 mole of (3-amino-1H-pyrazol-4-yl)-2-furanyl-methanone in 30 ml of glacial acetic acid was refluxed for 5 hours. The solvent was removed in vacuo and the residue partitioned between saturated aqueous sodium bicarbonate and dichloromethane. The dichloromethane layer was dried over sodium sulfate and passed through a short pad of hydrous magnesium silicate. The eluent was concentrated and the residue crystallized from dichloromethane:hexane to give the desired product as crystals, mp 228°-229° C.

WORKUP

后处理

  1. temperaturewas refluxed for 5 hours
  2. customThe solvent was removed in vacuo
  3. customthe residue partitioned between saturated aqueous sodium bicarbonate and dichloromethane
  4. dry with materialThe dichloromethane layer was dried over sodium sulfate
  5. concentrationThe eluent was concentrated
  6. customthe residue crystallized from dichloromethane