反应详情

温度

80 °C

To methyl 5-bromo-thiophene-2-carboxylate (2 g), tri-2-furylphosphine (400 mg), and tris(dibenzylidineacetone)dipalladium(0) (400 mg) was added DMF (50 mL), 2-(tributylstannyl)pyridine (4 g) and TEA (1 mL) The mixture was heated at 80° C. for 7 hours, cooled and partitioned between ethyl acetate and brine. The aqueous phase was extracted with ethyl acetate, and the extract was dried, filtered and concentrated. The concentrate was flash chromatographed on silica gel with a 20-70% ethyl acetate in hexane.

1. temperaturecooled
2. custompartitioned between ethyl acetate and brine
3. extractionThe aqueous phase was extracted with ethyl acetate
4. customthe extract was dried
5. filtrationfiltered
6. concentrationconcentrated
7. customchromatographed on silica gel with a 20-70% ethyl acetate in hexane