反应详情

温度

0 °C

3-Cyano-N-(2,4-dimethoxybenzyl)-4-[2-pyridazin-4-yl-4-(trifluoromethyl)benzyl]-N-1,2,4-thiadiazol-5-ylbenzenesulfonamide (Preparation 34, 54 mg, 0.083 mmol) was dissolved in dichloromethane (0.75 mL) and cooled to 0° C. Trifluoroacetic acid (32 μL, 0.41 mmol) was added as a solution in dichloromethane (0.25 mL) and the reaction stirred for 2 hours warming slowly to room temperature. The solvent was removed in vacuo and the residue re-dissolved in methanol. Once again the solvent was removed in vacuo. The material was suspended in methanol and filtered through Celite™. The reaction mixture was concentrated in vacuo and purified by the basic preparative HPLC method to afford the title compound.

1. temperaturewarming slowly to room temperature
2. customThe solvent was removed in vacuo
3. dissolutionthe residue re-dissolved in methanol
4. customOnce again the solvent was removed in vacuo
5. filtrationfiltered through Celite™
6. concentrationThe reaction mixture was concentrated in vacuo
7. custompurified by the basic preparative HPLC method