反应详情

温度

100 °C

Potassium carbonate (0.58 g, 4.14 mmol) was added to a sealed tube containing a solution of 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-methyl-1H-pyrazole-3-carbonitrile (1.0 g, 2.76 mmol) obtained in Step 2, hydroxylamine hydrochloride (0.39 g, 5.52 mmol) dissolved in MeOH (16 mL). The mixture was stirred vigorously and heated at 100° C. for 16 hr. The white precipitate formed was filtered and washed twice with cold water. It was further dried under a high vacuum. The filtrate was extracted with chloroform (30 mL×2), dried over MgSO4, filtered and evaporated under a vacuum, to obtain the title product in a compound amount of 1.04 g (2.63 mmol, 95%).

1. customThe white precipitate formed
2. filtrationwas filtered
3. washwashed twice with cold water
4. customIt was further dried under a high vacuum
5. extractionThe filtrate was extracted with chloroform (30 mL×2)
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. customevaporated under a vacuum