反应详情

A solution of 3-methylisoquinoline (5.4 g, 0.04 mol) in concentrated sulfuric acid (30 ml) was cautiously added to a solution of potassium nitrate (4.25 g, 1.1 eq) in concentrated sulfuric acid (23 ml) whilst maintaining the temperature below 4° C. (ice bath). Stirring was continued for 2 h and then temperature raised to ambient. Reaction was further stirred for 3 h and then poured into ice-water slurry (500 mL. Neutralisation using solid potassium carbonate affored a yellow solid which was filtered and washed with water. This material was dissolved in ethanol (200 mL, filtered and concentrated under reduced pressure to afford the title compound as a yellow solid.

1. temperaturewhilst maintaining the temperature below 4° C. (ice bath)
2. temperaturetemperature raised to ambient
3. customReaction
4. stirringwas further stirred for 3 h
5. filtrationwas filtered
6. washwashed with water
7. dissolutionThis material was dissolved in ethanol (200 mL
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure