反应详情

3,4-Difluorothiophenol (0.101 g, 0.690 mmol) and potassium carbonate (0.200 g, 1.45 mmol) were stirred in N,N-dimethylacetamide (3 mL). After 5 minutes, 3-cyano-N-(2,4-dimethoxybenzyl)-4-fluoro-N-1,2,4-thiadiazol-5-ylbenzenesulfonamide (Preparation 1, 0.300 g, 0.690 mmol) was added to the reaction mixture and the mixture stirred at ambient temperature overnight. The mixture was partitioned between ethyl acetate and water. The organic layer was washed with a 1M aqueous solution of sodium hydroxide, followed by brine, then dried over MgSO4, filtered and concentrated in vacuo to give a white solid. The solid was then dissolved in 1,4-dioxane and a 4M solution of hydrogen chloride in 1,4-dioxane (3 mL) added. The reaction mixture was stirred at ambient temperature overnight. The reaction mixture was concentrated in vacuo to give a residue. The residue was solubilised in dimethylsulfoxide (1 mL) and purified by the B-HPLC method to afford the title compound.

1. customThe mixture was partitioned between ethyl acetate and water
2. washThe organic layer was washed with a 1M aqueous solution of sodium hydroxide
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customto give a white solid
7. stirringThe reaction mixture was stirred at ambient temperature overnight
8. concentrationThe reaction mixture was concentrated in vacuo
9. customto give a residue
10. custompurified by the B-HPLC method