HRID867054

反应详情

EQUATION

反应方程式

HRID 867054 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of phenoxycarbonylisocyanate (7.0 g., 0.043 mole) in 50 ml. of dioxane is added 4-aminoveratrole (6.57 g., 0.043 mole) under a nitrogen atmosphere while maintaining a temperature of 20°-25°. Following the addition of the 4-aminoveratrole, a second 50 ml. portion of dioxane is added and the solution refluxed for a period of one hour. Concentration of the reaction mixture under reduced pressure provides an oily solid residue. Titration of this residual material with about 40 ml. of cold carbon tetrachloride followed by crystallization from acetonitrile provides analytically pure 1-(3,4-dimethoxyphenyl)-3-phenoxycarbonylurea, m.p. 139.5°-142°.

WORKUP

后处理

  1. temperaturewhile maintaining a temperature of 20°-25°
  2. temperaturethe solution refluxed for a period of one hour
  3. customConcentration of the reaction mixture under reduced pressure provides an oily solid residue
  4. customof cold carbon tetrachloride followed by crystallization from acetonitrile