反应详情

A solution of 5-fluoro-2-nitrobenzoic acid (10.0 g, 54 mmol, 1.0 equiv.), 2-amino-5-chloropyridine (9.02 g, 1.3 equiv.), in 80 mL of pyridine was treated with phosphorous oxychloride (25.3 g, 3.0 equiv.) for 30 minutes. The volatile was evaporated and the residue was redissolved into EtOAc, washed with 1N HCl, saturated aqueous NaHCO3 and saturated aqueous NaCl. The organic layer was dried over Na2SO4, filtered, and evaporated. The product was triturated with diethyl ether to give N-(5-chloro-2-pyridinyl)-(2-nitro)-5-fluorophenylcarboxamide (11.5 g, 72%). MS found for C12H7ClFN3O'(M+H)+: 296, (M+2+H): 298.

1. customThe volatile was evaporated
2. dissolutionthe residue was redissolved into EtOAc
3. washwashed with 1N HCl, saturated aqueous NaHCO3 and saturated aqueous NaCl
4. dry with materialThe organic layer was dried over Na2SO4
5. filtrationfiltered
6. customevaporated
7. customThe product was triturated with diethyl ether