HRID1696334
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 6-methoxy-2,2-dimethyl-3,4-dihydronaphthalen-1(2H)-one (3.30 g, 16.2 mmol) and 1-bromopyrrolidine-2,5-dione (2.88 g, 16.2 mmol) in 50 mL of CCl4, was added AIBN (0.265 g, 1.62 mmol). The mixture was heated to reflux for three hours. The reaction was cooled to RT and the reaction was quenched with water (25 mL) and extracted with EtOAc (3×100 mL). The combined organic layers were washed with brine, dried over MgSO4 and filtered. The solvent was evaporated and the residue was purified by column chromatography (0-50% EtOAc/Hexane to provide the title compound as a white solid (3.92 g, 86% yield). MS m/z: 284.2 (M+1).
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureto reflux for three hours
- customthe reaction was quenched with water (25 mL)
- extractionextracted with EtOAc (3×100 mL)
- washThe combined organic layers were washed with brine
- dry with materialdried over MgSO4
- filtrationfiltered
- customThe solvent was evaporated
- customthe residue was purified by column chromatography (0-50% EtOAc/Hexane