HRID1588730
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
To a mixture of 4-acetoxy-3,5-dimethoxybenzoic acid (672 mg), diphenylphosphoryl azide (990 mg) and benzene (15 ml) was dropwise added triethylamine (0.42 ml), while stirring. The mixture was stirred for 20 minutes at room temperature and further for 30 minutes under refluxing to obtain a solution of 4-acetoxy-3,5-dimethoxyphenyl isocyanate in benzene. 3-Amino-4-(2-chlorophenyl)-1,6,7-trimethyl-2(1H)-quinolone (624 mg) was added to the above solution and the mixture was refluxed for 2.5 hours. The mixture was washed with water, aqueous sodium hydrogen carbonate solution, water, diluted hydrochloric acid and then water in this order, dried (MgSO4) and concentrated.
WORKUP
后处理
- stirringThe mixture was stirred for 20 minutes at room temperature and further for 30 minutes
- temperatureunder refluxing