反应详情

A stirred mixture of 4-(3-chloro-4-fluoroanilino)-7-chloro-6-nitro-3-quinolinecarbonitrile (1.88 g, 5.0 mmol), N-methylpiperazine (5 ml, 45 mmol), and 10 ml of toluene was refluxed for 45 m, evaporated to remove volatile matter, and stirred in water with potassium carbonate (2.75 g). The resulting solid was filtered, washed with water, and dried to give 2.26 g. An acetone solution was passed onto a pad of silica gel; elution with 50:2:1 acetone-MeOH-TEA and evaporation gave a red solid, mp 240-246°; ms 441.2 (M+H)+, 221.2 (M+2H)+2.

1. temperaturewas refluxed for 45 m
2. customevaporated
3. customto remove volatile matter
4. filtrationThe resulting solid was filtered
5. washwashed with water
6. customdried
7. customto give 2.26 g
8. washelution
9. customwith 50:2:1 acetone-MeOH-TEA and evaporation
10. customgave a red solid, mp 240-246°