反应详情

To 4 g verapamil (8.8 mmole) in 100 ml of benzene was added to 2.2 g of palladium acetate. The mixture was stirred for four days at room temperature. A saturated solution of NaCl in 100 ml of water and 96 ml of acetone was added to the resulting mixture, which was stirred at room temperature for 15 minutes. Solvent was then removed under reduced pressure. Then, there was added to the mixture 100 ml of toluene, 25 ml of triethylamine and 10 mmol of methylvinylketone. The mixture was heated at 120° C. for 2 hours, and then allowed to cool to room temperature. The organic phase was filtered, washed with water, dried, filtered again and solvent was removed. After separation by chromatography, the title compound was obtained (3.2 g, 80%) [m.p. 119-121, from ether].

1. stirringwas stirred at room temperature for 15 minutes
2. customSolvent was then removed under reduced pressure
3. temperatureThe mixture was heated at 120° C. for 2 hours
4. temperatureto cool to room temperature
5. filtrationThe organic phase was filtered
6. washwashed with water
7. customdried
8. filtrationfiltered again
9. customsolvent was removed
10. customAfter separation by chromatography