HRID1417995

反应详情

EQUATION

反应方程式

HRID 1417995 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

A mixture of 4-chloro-6-(3'-methylanilino)pyrimidine (9.56 g) and 3-aminophenol (5.22 g) was stirred and heated at 140° C. for 3 hours. The product so obtained was dissolved in methylene chloride and a few drops of methanol, and chromatographed on silica using a mixture of methylene chloride and methanol, increasing in polarity from pure methylene chloride to a 19:1 mixture of methylene chloride and methanol as eluent. The product so obtained was recrystallised from a mixture of ethyl acetate and hexane to give 4-(3'-hydroxyanilino)-6-(3'-methylanilino)pyrimidine in 39% yield, m.p. 188°-189° C.;

WORKUP

后处理

  1. customThe product so obtained
  2. customa few drops of methanol, and chromatographed on silica using
  3. additiona mixture of methylene chloride and methanol
  4. temperatureincreasing in polarity from pure methylene chloride to a 19:1 mixture of methylene chloride and methanol as eluent
  5. customThe product so obtained
  6. customwas recrystallised from a mixture of ethyl acetate and hexane