反应详情

5-Chloro-N-(2,4-dimethoxybenzyl)-2,4-difluoro-N-(5-fluoropyridin-2-yl)benzenesulfonamide (Preparation 105, 23 mg, 0.04 mmol), 3-(1-methyl-1H-pyrazol-5-yl)biphenyl-4-ol (Preparation 107, 9 mg, 0.04 mmol) and potassium carbonate (15 mg, 0.11 mmol) in dimethyl sulfoxide (1 mL) were stirred at room temperature for 2 hours. The mixture was treated with aqueous 2M HCl (3 mL). The resulting mixture was extracted with dichloromethane (3 mL). The dichloromethane layer was dried through a phase separating cartridge followed by treatment with trifluoroacetic acid (500 μL). The mixture was stirred for 2 hours and allowed to stand at room temperature for 18 hours. The mixture was then treated with a saturated solution of ammonium chloride (5 mL). The dichloromethane layer was separated, dried through a phase separating cartridge and evaporated in vacuo. The residue was purified by preparative HPLC to afford the title compound (14 mg, 45%).

1. extractionThe resulting mixture was extracted with dichloromethane (3 mL)
2. dry with materialThe dichloromethane layer was dried through a phase
3. customseparating cartridge
4. waitto stand at room temperature for 18 hours
5. additionThe mixture was then treated with a saturated solution of ammonium chloride (5 mL)
6. customThe dichloromethane layer was separated
7. customdried through a phase
8. customseparating cartridge
9. customevaporated in vacuo
10. customThe residue was purified by preparative HPLC