反应详情

To a suspension of 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-methylsulfinylpyrazole (20 g) in methanol (120 ml) was added hydroxylamine hydrochloride (3.99 g), followed by addition of triethylamine (8.0 ml). The mixture was stirred at room temperature overnight then evaporated. The residue was partitioned between water and ethyl acetate. The organic layer was washed with water, followed by wash with brine. The organic layer was dried over anhydrous sodium sulfate. The solution was concentrated by evaporation of solvent. A precipitate was formed and collected by filtration. The solid was washed with small amount of ethyl acetate to give Compound 44 (16.1 g), m.p. 225-226° C.

1. customthen evaporated
2. customThe residue was partitioned between water and ethyl acetate
3. washThe organic layer was washed with water
4. washby wash with brine
5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
6. concentrationThe solution was concentrated by evaporation of solvent
7. customA precipitate was formed
8. filtrationcollected by filtration
9. washThe solid was washed with small amount of ethyl acetate