反应详情

Dissolved 5-amino-3-((3-chlorophenyl)amino)-1H-pyrazole-4-carbonitrile in DMSO (40 mL), added potassium carbonate (0.50 eq, 2.59 g), then added hydrogen peroxide solution (3.5 mL of 30% solution in deionized water) dropwise over ice bath over the course of 10 minutes. After the final addition, kept on ice bath for 2 h, then heated to room temperature and stirred until complete by TLC. After 24 h, reaction had not come to completion, so the amount of hydrogen peroxide was doubled (additional 3.5 mL). Still incomplete, though progressing, the reaction was stirred at room temperature over the weekend. Reaction was complete by TLC after 3 days of stirring and was poured into 350 mL of ice water. After precipitate formed, solution was filtered and washed with water to obtain 5-amino-3-((3-chlorophenyl)amino)-1H-pyrazole-4-carboxamide as gray powder.

1. customover the course of 10 minutes
2. additionAfter the final addition
3. waitAfter 24 h
4. customreaction
5. stirringStill incomplete, though progressing, the reaction was stirred at room temperature over the weekend
6. customReaction
7. waitwas complete by TLC after 3 days
8. stirringof stirring
9. customAfter precipitate formed
10. filtrationsolution was filtered
11. washwashed with water