HRID1766660
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 solution of 6-[2-methoxy-5-(5-methyl-7-nitroindan-4-yloxy)benzyl]-2H-pyridazine-3-one (704 mg) in acetic acid (10 mL) was added hydrobromic acid (48%, 10 mL). The mixture was heated at reflux temperature under an argon atmosphere overnight. After adding water, the reaction mixture was extracted with dichloromethane. The organic layer was washed with water and brine successively, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure. The residue was crystallized from a small amount of ethyl acetate to give the title compound (270 mg).
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureat reflux temperature under an argon atmosphere overnight
- extractionthe reaction mixture was extracted with dichloromethane
- washThe organic layer was washed with water and brine successively
- dry with materialdried over anhydrous magnesium sulfate
- customThe solvent was removed under reduced pressure
- customThe residue was crystallized from a small amount of ethyl acetate