反应详情

To a solution of 2-amino-3-cyanopyridine (1.00 g, 8.40 mmol) in pyridine (8 mL) and TEA (0.8 mL) in a sealed tube, H2S gas was bubbled through for 5 min. It was then stirred at room temperature for 20 h. The mixture was concentrated in vacuo to dryness. The residue was dissolved in MeOH (10 mL). To the solution, aq. H2O2 (30%, 3 mL) was added. The mixture was then stirred at room temperature for 5 h, during which time, solids precipitated out. The solids were collected by filtration, dried on vacuum to give isothiazolo[3,4-b]pyridin-3-amine (860 mg).

1. concentrationThe mixture was concentrated in vacuo to dryness
2. dissolutionThe residue was dissolved in MeOH (10 mL)
3. additionTo the solution, aq. H2O2 (30%, 3 mL) was added
4. stirringThe mixture was then stirred at room temperature for 5 h, during which time, solids
5. customprecipitated out
6. filtrationThe solids were collected by filtration
7. customdried on vacuum