反应详情

温度

40 °C

A solution of 1-[(7-benzyloxy-3-nitroquinolin-4-yl)amino]-2-methylpropan-2-ol (245.0 g, 0.667 mol) in methanol (3 L) was added to a pressure vessel containing 5% platinum on carbon (7.35 g). The vessel was placed under hydrogen pressure (30 psi, 2.1×105 Pa) at 55° C. for five hours. The reaction was allowed to cool to 40° C., and dichloromethane (2.5 L) was added. The reaction mixture was then filtered through CLARCEL filter aid at 30-40° C., and the filter cake was washed with methanol. The filtrate was concentrated to a volume of 1.5 L, cooled to 5-10° C., and stirred for two hours. A solid formed and was isolated by filtration, washed with a small amount of methanol, and dried under vacuum at 50° C. to provide 199.4 g of 1-{[3-amino-7-(benzyloxy)quinolin-4-yl]amino}-2-methylpropan-2-ol.

1. customat 55° C.
2. customfor five hours
3. filtrationThe reaction mixture was then filtered through CLARCEL
4. filtrationfilter aid at 30-40° C.
5. washthe filter cake was washed with methanol
6. concentrationThe filtrate was concentrated to a volume of 1.5 L
7. temperaturecooled to 5-10° C.
8. customA solid formed
9. customwas isolated by filtration
10. washwashed with a small amount of methanol
11. customdried under vacuum at 50° C.