反应详情

To a refluxing mixture of 4-acetylbiphenyl (20 g), I2 (5 mg) and Zn (6.8 g) in benzene (200 ml) was added ethylbromoacetate (12 ml) dropwise during 30 minutes. The mixture was refluxed for 1 h and then cooled to room temperature. It was acidified with 10% HCl (100 ml) and benzene layer was separated out. The organic layer was washed with water, dried (Na2SO4) and concentrated. The crude product was purified by column chromatography on silica gel to give 20.6 g (72.1% yield) of ethyl 3-hydroxy-3-([1,1′-biphenyl]-4yl)butanoate (2e, formula 2, R=Ph) m.p. 58-60° C.

1. temperatureThe mixture was refluxed for 1 h
2. customwas separated out
3. washThe organic layer was washed with water
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated
6. customThe crude product was purified by column chromatography on silica gel