反应详情

A mixture of 5-bromonicotinamide (2.5 g, 12.4 mmol), tributyl(1-ethoxyvinyl)tin (5.0 g, 13.8 mmol) and dichlorobis(triphenylphosphine)palladium(II) (800 mg, 1.1 mmol) in 25 mL toluene was heated to reflux for 3 hours. The mixture was cooled to room temperature, treated with 25 mL 2N HCl (aq.), and stirred for 1 hour. The aqueous layer was washed with ethyl acetate, adjusted to pH >7 with solid K2CO3, and extracted six times into 20% isopropanol/chloroform. The combined extracts were dried (Na2SO4), filtered, and concentrated to provide the desired product (1.6 g, 78%).

1. temperaturewas heated
2. temperatureto reflux for 3 hours
3. washThe aqueous layer was washed with ethyl acetate
4. extractionextracted six times into 20% isopropanol/chloroform
5. dry with materialThe combined extracts were dried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated