反应详情

Benzo[b]quinolizinium bromide (508.5 g, 1.95 mol) was dissolved in 5 L of distilled water with heating (steam-bath). Potassium hexafluorophosphate (367.2 g, 1.95 mol) was dissolved in 1.1 L of water with heating and the resulting solution was poured in portions into the above bromide solution with steam-bath heating (20 min). The precipitate was formed immediately and the mixture was stirred at room temperature for 3 h, then stirred 1 h in an ice-water bath. The solid was filtered, washed with cold water (800 mL), dried (50°-60° C.) in vacuo for 3 days to afford 601 g (94.8%) of benzo[b]quinolizinium hexafluorophosphate. (Formula lI: R1 =R2 =R7 =H; X- --=PF6-).

1. temperaturewith heating (steam-bath)
2. temperaturewith heating
3. temperatureheating (20 min)
4. customThe precipitate was formed immediately
5. stirringstirred 1 h in an ice-water bath
6. filtrationThe solid was filtered
7. washwashed with cold water (800 mL)
8. customdried (50°-60° C.) in vacuo for 3 days