HRID1857227
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-(6,7-Dimethoxy-4-quinolyl)-2-(4-bromophenyl)acetonitrile (850 mg) obtained in Example 161 was dissolved in 60% aqueous sulfuric acid (5 ml), and the solution was refluxed with heat for 1 hour and then poured into a container with ice and aqueous ammonia. The solution was neutralized with hydrochloric acid and extracted with methylene chloride. After drying with anhydrous sodium sulfate and removing the solvent by distillation, the resulting residue was purified by column chromatography on silica gel eluting with chloroform/methanol (100/1) to obtain 260 mg of the title compound (yield: 33%).
WORKUP
后处理
- temperaturethe solution was refluxed
- temperaturewith heat for 1 hour
- extractionextracted with methylene chloride
- dry with materialAfter drying with anhydrous sodium sulfate
- customremoving the solvent
- distillationby distillation
- customthe resulting residue was purified by column chromatography on silica gel eluting with chloroform/methanol (100/1)