HRID1247947
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas refluxed for 5 hours
- customThe solvent was removed in vacuo
- customthe residue partitioned between saturated aqueous sodium bicarbonate and dichloromethane
- dry with materialThe dichloromethane layer was dried over sodium sulfate
- concentrationThe eluent was concentrated
- customthe residue crystallized from dichloromethane