HRID895500

反应详情

EQUATION

反应方程式

HRID 895500 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a crude sample of N-(6-chloro-2-phenylpyrimidin-4-yl)-2-{4-[(2E)-3-phenylprop-2-enyl]piperazin-1-yl}acetamide (22.54) (0.75 g in 60 ml DMSO) were added glycinamide hydrochloride (1.85 g in 10 ml DMSO) and N,N-diisopropylethylamine (2.96 ml) and the mixture heated to 100° C. for 16 hrs. The solvent was then removed in vacuo and the residue purified twice by flash chromatography on silica gel using mixtures of dichloromethane and methanol (97:3, 95:5 then 93:7 v/v/v). Further purification by recrystallization from methanol furnished the title compound (32 mg over 2 steps).

WORKUP

后处理

  1. customThe solvent was then removed in vacuo
  2. customthe residue purified twice by flash chromatography on silica gel using mixtures of dichloromethane and methanol (97:3, 95:5
  3. customFurther purification
  4. customby recrystallization from methanol