HRID1672343

反应详情

EQUATION

反应方程式

HRID 1672343 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 0.644 g (3.939 mmol) benzoyl isocyanate in 10 ml CH2Cl2 is added within 10 min to 1 g (3.029 mmol) of 8-chloro-1-(2-chloro-phenyl)-1H-imidazo[4,5-c]quinoline 5-oxide (Example 71) in 10 ml CH2Cl2. The reaction mixture is heated and kept under reflux for 7 h. The solvent is evaporated, and the residue is purified by chromatography (CH2Cl2-methanol 97.5:2.5). The compound is crystallized from ethyl acetate-hexane. mp: 255-258° C.; MS: 433 (M++1); HPLC: tret=10.91 min (Grad 1).

WORKUP

后处理

  1. temperatureThe reaction mixture is heated
  2. temperatureunder reflux for 7 h
  3. customThe solvent is evaporated
  4. customthe residue is purified by chromatography (CH2Cl2-methanol 97.5:2.5)
  5. customThe compound is crystallized from ethyl acetate-hexane
  6. customtret=10.91 min (Grad 1)