反应详情

Intermediate 1 (20 g) was added to a stirred solution of 2-bromobenzonitrile (10.34 g) and tetrakis(triphenylphosphine)palladium (0) (1.5 g) in DME (200 ml) and 8% NaHCO3 (50 ml) at reflux under nitrogen. Further catalyst (1.5 g) was added and the reaction continued overnight. The reaction was cooled to room temperature and diluted with ether (200 ml). The organic layer was separated, washed with water (3×100 ml) and dried. Filtration and evaporation gave a white solid which was purified by chromatography eluting with System A (1:9) to give the title compound (10.58 g) as a white solid. T.l.c. System A (1:9), Rf 0.45.

1. temperatureat reflux under nitrogen
2. customthe reaction continued overnight
3. customThe organic layer was separated
4. washwashed with water (3×100 ml)
5. customdried
6. filtrationFiltration and evaporation
7. customgave a white solid which
8. customwas purified by chromatography
9. washeluting with System A (1:9)