反应详情

A mixture of (5-methoxy-3-methyl-1-oxo-3,4-dihydro-1H-naphthalen-2-ylidene)-acetic acid ethyl ester (480 mg), NBS (420 mg), and AIBN (30 mg) in CCl4 (18 mL) was refluxed for 3 hours. The reaction mixture was then cooled to room temperature, quenched with saturated sodium bicarbonate solution and extracted with dichloromethane (2×). The combined organics were washed with water, dried (Na2SO4), concentrated, and purified by flash column chromatography to give a light brown solid (420 mg) LCMS-ESI+ (m/z): [M+H]+ calcd for C16H18BrO4: 353.03. Found: 352.91.

1. temperaturewas refluxed for 3 hours
2. customquenched with saturated sodium bicarbonate solution
3. extractionextracted with dichloromethane (2×)
4. washThe combined organics were washed with water
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated
7. custompurified by flash column chromatography