反应详情

3-Cyano-N-(2,4-dimethoxybenzyl)-4-{[3-pyridazin-4-yl-3′-(trifluoromethyl)biphenyl-4-yl]oxy}-N-1,2,4-thiadiazol-5-ylbenzenesulfonamide (Preparation 20, 386 mg, 0.52 mmol) was dissolved in a 4M solution of hydrogen chloride in 1,4-dioxane (13 mL) and stirred at room temperature for 18 hours. The reaction was concentrated in vacuo and purified using silica gel column chromatography (1% acetic acid in dichloromethane to 10% methanol and 1% acetic acid in dichloromethane gradient elution) followed by a second purification using silica gel column chromatography (0%-15% methanol in dichloromethane gradient elution) to afford the title compound (76 mg, 25%).

1. concentrationThe reaction was concentrated in vacuo
2. custompurified
3. washsilica gel column chromatography (1% acetic acid in dichloromethane to 10% methanol and 1% acetic acid in dichloromethane gradient elution)
4. customfollowed by a second purification
5. washsilica gel column chromatography (0%-15% methanol in dichloromethane gradient elution)