HRID2352161

反应详情

EQUATION

反应方程式

HRID 2352161 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureat reflux for 24 hours
  2. customThe solvent was evaporated to 1/3 volume
  3. temperaturethe mixture was cooled in an ice-bath
  4. customto crystallize the crude product
  5. filtrationThe product was collected by filtration
  6. washwashed with water
  7. customThe material was recrystallized from isopropanol/ethylene glycol monomethyl ether