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
{2-Amino-5-[(6,7-dimethoxy-4-quinolyl)oxy]phenyl}methanol (63 mg) was dissolved in heated triethylamine/toluene (1.2 ml/6 ml) to prepare a solution. Triphosgene (98 mg) was added to the solution and was heated under reflux for 2 min. The reaction solution was cooled to room temperature, water was then added to the reaction solution, and the mixture was extracted with chloroform. The chloroform layer was then washed with water and saturated brine and was dried over anhydrous sodium sulfate. The solvent was removed therefrom by distillation under the reduced pressure, and the residue was purified by column chromatography on silica gel using acetone-chloroform to give the title compound (24 mg, yield 39%).
WORKUP
后处理
- customto prepare a solution
- temperaturewas heated
- temperatureunder reflux for 2 min
- extractionthe mixture was extracted with chloroform
- washThe chloroform layer was then washed with water and saturated brine
- dry with materialwas dried over anhydrous sodium sulfate
- customThe solvent was removed
- distillationby distillation under the reduced pressure
- customthe residue was purified by column chromatography on silica gel