HRID2352161
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 14.4 g amount of 3-dimethylamino-1-(4-pyridinyl)-2-propen-1-one (U.S. Pat. No. 4,281,000) and 16.1 g of 4-methoxyphenylguanidine carbonate in 200 ml of isopropanol was heated at reflux for 24 hours. The solvent was evaporated to 1/3 volume, then the mixture was cooled in an ice-bath to crystallize the crude product. The product was collected by filtration and washed with water, then with isopropanol. The material was recrystallized from isopropanol/ethylene glycol monomethyl ether to give 16.7 g of the desired product as yellow crystals, mp 174°-175° C.
WORKUP
后处理
- temperatureat reflux for 24 hours
- customThe solvent was evaporated to 1/3 volume
- temperaturethe mixture was cooled in an ice-bath
- customto crystallize the crude product
- filtrationThe product was collected by filtration
- washwashed with water
- customThe material was recrystallized from isopropanol/ethylene glycol monomethyl ether