反应详情

Sodium acetate (7.4g) was added to a mixture of hydroxylamine hydrochloride (6.3 g) and 3-cyclopropyl-2-ethoxymethylene-1-(2-fluoro-4-methylsulphonylphenyl)-propan-1,3-dione (29.0g) in ethanol. The mixture was stirred at room temperature overnight. The solvent was evaporated and the residue was partitioned between ethyl acetate and water. The organic phase was washed with water, dried (anhydrous magnesium sulphate) filtered and evaporated to dryness. The residue was triturated with ether and filtered. The resultant solid was recrystallized from methanol. The mother liquors from the recrystallization were combined and evaporated to dryness. The residue was purified by column chromatography on silica gel to give 4-cyclopropylcarbonyl-5-(2-fluoro-4-methylsulphonylphenyl)-isoxazole (compound 1) as a white solid, m.p. 129.5°-130.5° C.

1. customThe solvent was evaporated
2. customthe residue was partitioned between ethyl acetate and water
3. washThe organic phase was washed with water
4. dry with materialdried (anhydrous magnesium sulphate)
5. filtrationfiltered
6. customevaporated to dryness
7. customThe residue was triturated with ether
8. filtrationfiltered
9. customThe resultant solid was recrystallized from methanol
10. customThe mother liquors from the recrystallization
11. customevaporated to dryness
12. customThe residue was purified by column chromatography on silica gel