HRID1672343
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction mixture is heated
- temperatureunder reflux for 7 h
- customThe solvent is evaporated
- customthe residue is purified by chromatography (CH2Cl2-methanol 97.5:2.5)
- customThe compound is crystallized from ethyl acetate-hexane
- customtret=10.91 min (Grad 1)