HRID1863007

反应详情

EQUATION

反应方程式

HRID 1863007 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of 1.30 g (0.0114 mol) of 2-chloropyrimidine, 3.50 g (0.00875 mol) of 1-[4-[[7-(trifluoromethyl)-4-quinolinyl]amino]benzoyl]piperazine, and 1.2 g of triethylamine in 50 ml of ethanol is stirred at 50° C. for 15 hours and at reflux for 8 hours. The mixture is partitioned between methylene chloride and aqueous 1 N sodium hydroxide. The organic phase is dried and concentrated. The residue is re-crystallized from methylene chloride and ethanol to yield 4.00 g of 4-(2-pyrimidinyl)-1-[4-[[7-(trifluoromethyl)-4-quinolinyl]amino]benzoyl]piperazine, of melting point 246°-247.5° C.

WORKUP

后处理

  1. temperatureat reflux for 8 hours
  2. customThe mixture is partitioned between methylene chloride and aqueous 1 N sodium hydroxide
  3. customThe organic phase is dried
  4. concentrationconcentrated
  5. customThe residue is re-crystallized from methylene chloride and ethanol