反应详情

温度

26 °C

Charge (2,6-difluoro-phenyl)-[4-(6-methyl-5-nitro-pyridin-2-yl)-piperazin-1-yl]-methanone (1.00 equiv, 1.44 moles, 520.00 g), methanol (197.66 moles, 8.00 L, 6.33 kg), and THF wetted 5% palladium on carbon (75.00 g) to a three gallon autoclave. Hydrogenate the reaction at 50 psi at room temperature while maintaining a temperature below 30° C. After 0.5 hours, cool to 26° C., and maintain for 2 hours. Filter and concentrate under reduced pressure. Filter to obtain solids, rinse with methanol then heptanes. An additional filtration yields a second batch of [4-(5-amino-6-methyl-pyridin-2-yl)-piperazin-1-yl]-(2,6-difluoro-phenyl)-methanone. Dry under reduced pressure at 45° C. (445 g).

1. customthe reaction at 50 psi at room temperature
2. temperaturewhile maintaining a temperature below 30° C
3. temperaturemaintain for 2 hours
4. filtrationFilter
5. concentrationconcentrate under reduced pressure
6. filtrationFilter
7. customto obtain solids
8. washrinse with methanol
9. filtrationAn additional filtration