HRID1417982

反应详情

EQUATION

反应方程式

HRID 1417982 的结构方程式

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 6-chloro-4-[4'-(2-hydroxyethoxy)anilino]pyrimidine (1.0 g), 3-methylaniline (5 ml) and NMP (20 ml) was stirred and heated to 140° C. for 72 hours. The mixture was cooled and partitioned between ethyl acetate and water. The precipitate was removed by filtration, the ethyl acetate fraction chromatographed on silica and the combined products extracted with boiling ethyl acetate. The product was recrystallised from a mixture of ethyl acetate and hexane to give 4-[4'-(2-hydroxyethoxy)anilino]6-(3'-methylanilino)pyrimidine in 20% yield, m.p. 196°-199° C.;

WORKUP

后处理

  1. temperatureThe mixture was cooled
  2. custompartitioned between ethyl acetate and water
  3. customThe precipitate was removed by filtration
  4. customthe ethyl acetate fraction chromatographed on silica
  5. extractionthe combined products extracted with boiling ethyl acetate
  6. customThe product was recrystallised from a mixture of ethyl acetate and hexane