反应详情

A mixture of intermediate 13 (0.009 mol) and pyridine (0.02 mol) in ethanol (80 ml) was stirred. A mixture of hydroxylamine-O-sulfonic acid (0.01 mol) in methanol (20 ml) was added. The mixture was stirred overnight. The solvent was evaporated. The residue was taken up in DCM. The organic solution was washed with a diluted NaOH solution and with water, dried, filtered and the solvent was evaporated. The residue was purified by column chromatography over silica gel (eluent:DCM). The pure fractions were collected and the solvent was evaporated. The residue was crystallized from 2-propanol. The precipitate was filtered off and dried, yielding 1 g (26%) of 3-(3-methyl-1,2,4-thiadiazol-5-yl)-6-[[4-[3-(trifluoromethyl)phenoxy]butyl]thio]pyridazine (compound 94).

1. additionwas added
2. stirringThe mixture was stirred overnight
3. customThe solvent was evaporated
4. washThe organic solution was washed with a diluted NaOH solution and with water
5. customdried
6. filtrationfiltered
7. customthe solvent was evaporated
8. customThe residue was purified by column chromatography over silica gel (eluent:DCM)
9. customThe pure fractions were collected
10. customthe solvent was evaporated
11. customThe residue was crystallized from 2-propanol
12. filtrationThe precipitate was filtered off
13. customdried