HRID736296

反应详情

EQUATION

反应方程式

HRID 736296 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-(5-(4-chloromethylbenzoylamino)-2-methylphenyl)-4-(3-pyridyl)-2-pyrimidine-amine (1 g, 2.33 mmol) was dissolved in tetrahydrofuran (20 ml), pyridine (360 ml, 4.66 mmol) was added thereto, and the mixture was stirred for 30 minutes. N-methylhomopiperazine (434 μl, 3.49 mmol) was added thereto, and the mixture was refluxed for 12 hours and filtered. The filtrate was concentrated, subjected to column chromatography (eluent: chloroform:methanol=3:1(v/v)), concentrated again, and then crystallized from dimethylether to give 4-(4-methylhomopiperazin-1-ylmethyl)-N-[4-methyl-3-(4-(pyridin-3-yl)pyrimidin-2-yl)aminophenyl]benzamide (0.71 g).

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 12 hours
  2. filtrationfiltered
  3. concentrationThe filtrate was concentrated
  4. concentrationconcentrated again
  5. customcrystallized from dimethylether