反应详情

Sodium acetate (1.1 g) was added to a solution of hydroxylamine hydrochloride (0.9 g) and 3-cyclopropyl-2-(N,N -dimethylaminomethylene)-1-[5-(methylsulphenyl)-pyrid-2-yl]propan-1,3-dione (3.24 g) in ethanol. The mixture was stirred for 1 hour then cooled and filtered. The solid was washed with cold ethanol and the filtrate was partially evaporated. Water was added and the mixture was stirred at 0° C. for 0.5 hours. It was extracted with dichoromethane washed with water, dried (Na2SO4) and filtered. The flitrate was evaporated to dryness and the residue was purified by chromatography eluted with mixture of ethyl acetate and hexane to give 4-cyclopropylcarbonyl-5-[5-(methylsulphenyl)pyrid-2-yl] isoxazole (compound 13, 0.41 g) as a white solid, m.p. 103°-104° C.

1. temperaturethen cooled
2. filtrationfiltered
3. washThe solid was washed with cold ethanol
4. customthe filtrate was partially evaporated
5. additionWater was added
6. stirringthe mixture was stirred at 0° C. for 0.5 hours
7. extractionIt was extracted with dichoromethane
8. washwashed with water
9. dry with materialdried (Na2SO4)
10. filtrationfiltered
11. customThe flitrate was evaporated to dryness
12. customthe residue was purified by chromatography
13. washeluted with mixture of ethyl acetate and hexane