反应详情

Potassium carbonate (0.220 g, 1.59 mmol) was added to a stirred solution of 2,5-difluoro-4-hydroxy-N-(methylsulfonyl)benzamide (Preparation 34, 0.200 g, 0.796 mmol) and 5-bromo-2-nitropyridine (0.170 g, 0.836 mmol) in DMSO (2.5 mL) at room temperature. The mixture was stirred at room temperature for 2 hours and then at 60° C. for 24 hours. The reaction mixture was partitioned between EtOAc and 2M aqueous HCl ensuring the water layer was acidic. The organic layer was separated and washed further with citric acid, water and brine, then dried over magnesium sulfate, filtered, evaporated in vacuo and triturated in diethyl ether to yield the title compound (0.180 g, 60%):

1. waitat 60° C. for 24 hours
2. customThe reaction mixture was partitioned between EtOAc and 2M aqueous HCl ensuring the water layer
3. customThe organic layer was separated
4. washwashed further with citric acid, water and brine
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. customevaporated in vacuo
8. customtriturated in diethyl ether