反应详情

3-amino-4-chloro-6,7-dimethoxyquinoline (3.3 g) was dissolved in tetrahydrofuran (70 ml) with stirring and then cooled in an ice/water bath to below 10° C. 48% aqueous fluoboric acid (7.3 ml) was then added and the mixture stirred for 5 minutes. A solution of sodium nitrite (1.05 g) in water (2 ml) was added keeping the temperature below 10° C. The reaction mixture was then stirred for 30 minutes with cooling. The resulting yellow solid was filtered off, washed with fresh tetrahydrofuran. Carefully vac dried. To give 4-chloro-6,7-dimethoxyquinoline-3-diazonium tetrafluoroborate (4.15 g, 89%).

1. temperaturecooled in an ice/water bath to below 10° C
2. stirringthe mixture stirred for 5 minutes
3. customthe temperature below 10° C
4. stirringThe reaction mixture was then stirred for 30 minutes
5. temperaturewith cooling
6. filtrationThe resulting yellow solid was filtered off
7. washwashed with fresh tetrahydrofuran