反应详情

Combine 7-Bromo-4-[2-(tetrahydropyran-2-yloxy)ethoxy]benzofuran (2.598 g, 7.61 mmol), bis(dibenzylideneacetone) palladium (0.461 g, 0.802 mmol), and 2-dicyclohexylphosphino-2-(N,N-dimethylamino)biphenyl (0.308 g, 0.783 mmol) in tetrahydrofuran (15 ml) under nitrogen. Add bromo(2-ethoxy-2-oxoethyl)zinc (2 equiv.), and heat the mixture at 80° C. for 16 hours. (Knochel, P.; Honed, P.; Eds. Organozinc Reagents: A Practical Approach; Oxford University Press, Inc: London, 1999). Cool the mixture to room temperature, filter through a silica plug eluting with ethyl ether, and concentrate. Purify by flash chromatography and elute with hexane:ethyl acetate to give 1.422 g (54%) of the title compound as an oil. Mass spectrum: electrospray (m/z) 265 (M++1-85).

1. filtrationfilter through a silica plug
2. washeluting with ethyl ether
3. concentrationconcentrate
4. customPurify by flash chromatography
5. washelute with hexane