HRID225499

反应详情

EQUATION

反应方程式

HRID 225499 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Chloroperoxybenzoic acid (Fluka, Buchs, Switzerland; 2.06 g of 55%, 4.27 mmol) is added to a stirred mixture of 4-[(4-methyl-1-piperazinyl)-methyl]-N-{4-methyl-3-[[4-(3-pyridinyl)-2-pyrimidinyl]-amino]-phenyl}-benzamide (prepared as described in EP 0 564 409 B1, Example 21; 2.00 g, 4.05 mmol) in dichloromethane (70 mL) at −20° C. The resulting mixture is then stirred at RT for 72 h. The solvent is then evaporated off under reduced pressure to yield a mixture which is purified by column chromatography on silica gel, eluent dichloromethane-methanol-water (70:30:5), to give the title compound as a yellow crystalline solid, m.p. 154-158° C.

WORKUP

后处理

  1. customThe solvent is then evaporated off under reduced pressure
  2. customto yield a mixture which
  3. customis purified by column chromatography on silica gel, eluent dichloromethane-methanol-water (70:30:5)