反应详情

温度

150 °C

A mixture of 4-chloro-1-{[3-(4-fluorophenyl)isoxazol-5-yl]methyl}-2-propyl-1H-imidazo[4,5-c]quinoline (0.806 g, 1.92 mmol) and 7 N ammonia in methanol (40 mL) was sealed in a pressure vessel and heated at 150° C. for 18 hours and allowed to cool to room temperature. The volatiles were removed under reduced pressure, and the resulting solid was stirred with 0.5 N sodium hydroxide in methanol. The solid was isolated by filtration, washed with diethyl ether, purified by column chromatography on silica gel (eluting with 5% to 10% CMA in chloroform), triturated with diethyl ether, isolated by filtration, and dried to provide 0.123 g of 1-{[3-(4-fluorophenyl)isoxazol-5-yl]methyl}-2-propyl-1H-imidazo[4,5-c]quinolin-4-amine as a white powder, mp 226.0-227.0° C.

1. customwas sealed in a pressure vessel
2. temperatureto cool to room temperature
3. customThe volatiles were removed under reduced pressure
4. customThe solid was isolated by filtration
5. washwashed with diethyl ether
6. custompurified by column chromatography on silica gel (eluting with 5% to 10% CMA in chloroform)
7. customtriturated with diethyl ether
8. customisolated by filtration
9. customdried