HRID1863022

反应详情

EQUATION

反应方程式

HRID 1863022 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 4-[4-[[7-(trifluoromethyl)-4-quinolinyl]amino]benzoyl]piperazine (2.0 g, 0.005 mol) in 15 ml of methylene chloride is added a solution of m-chlorophenyl isocyanate in 10 ml of methylene chloride at 0° C. under nitrogen. The resulting suspension is stirred for 1 hour at room temperature. The above mixture is then filtered and the white solid residue is washed with more methylene chloride and dried. This is recrystallized from methanol/methylene chloride to give 2.5 g (90%) of white crystalline 1-[[(3-chlorophenyl)amino]carbonyl]-4-[4-[[7-(trifluoromethyl)-4-quinolinyl]amino]benzoyl]piperazine of melting point 266°-268° C.

WORKUP

后处理

  1. filtrationThe above mixture is then filtered
  2. washthe white solid residue is washed with more methylene chloride
  3. customdried
  4. customThis is recrystallized from methanol/methylene chloride