反应详情

In formic acid (60 ml) was dissolved 3-(tert-butoxyamino)-4-mercaptopyridine (9.20 g), followed by heating under reflux for 4 hours. After the reaction mixture was concentrated under reduced pressure and a 5N aqueous solution (100 ml) of potassium hydroxide was added to the residue, the resulting mixture was extracted with ether. The organic layer was dried over anhydrous sodium sulfate and distilled under reduced pressure to remove the solvent. Diethyl ether was added to the residue and the solid so precipitated was collected by filtration, whereby the title compound was obtained as a colorless solid (3.97 g).

1. temperatureby heating
2. temperatureunder reflux for 4 hours
3. concentrationAfter the reaction mixture was concentrated under reduced pressure
4. additiona 5N aqueous solution (100 ml) of potassium hydroxide was added to the residue
5. extractionthe resulting mixture was extracted with ether
6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
7. distillationdistilled under reduced pressure
8. customto remove the solvent
9. additionDiethyl ether was added to the residue
10. customthe solid so precipitated
11. filtrationwas collected by filtration, whereby the title compound