反应详情

To a dichloromethane (10 mL) solution of 5-chloro-4-(6-cyclopropyl-5-(1,1-difluoroethoxy)pyridin-3-yloxy)-2-fluorobenzoic acid (Preparation 271, 220 mg, 0.57 mmol) was added methanesulfonamide (64 mg, 0.68 mmol), HATU (259 mg, 0.68 mmol), and DIPEA (0.35 mL, 1.99 mmol). The reaction was left to stir at room temperature for 2 hours. The reaction was washed with a 2M aqueous solution of HCl (50 mL) and extracted into DCM (3×50 mL). The combined organics were dried over MgSO4, filtered and the solvent removed to leave an off white solid. The solid was triturated in a minimum of methanol, filtered and dried in air, to leave the title compound as a white solid as the HCl salt. (131 mg, 50%).

1. waitThe reaction was left
2. washThe reaction was washed with a 2M aqueous solution of HCl (50 mL)
3. extractionextracted into DCM (3×50 mL)
4. dry with materialThe combined organics were dried over MgSO4
5. filtrationfiltered
6. customthe solvent removed
7. customto leave an off white solid
8. customThe solid was triturated in a minimum of methanol
9. filtrationfiltered
10. customdried in air