反应详情

温度

80 °C

A solution of 2-fluoro-4-bromobenzonitrile in DMF is treated with potassium acetate, bispinacolatoboronate (1.1 equiv.) and catalytic PdCl2(dppf) and heated for 2 h at 80° C. The reaction mixture is cooled to room temperature and 4-bromonicotinic acid (1 equiv.) is added along with fresh catalyst and 2 M Na2CO3 and the resulting mixture is stirred at 80° C. for 18 h. Solvent is removed and the residue is treated with 4N HCl/dioxane in refluxing ethanol for 18 h. The reaction is evaporated and the residue in ethyl acetate is washed with NaHCO3 (aqueous), dried over MgSO4 and evaporated to give 5-(4-cyano-3-fluoro-phenyl)-nicotinic acid ethyl ester.

1. temperatureThe reaction mixture is cooled to room temperature
2. customSolvent is removed
3. additionthe residue is treated with 4N HCl/dioxane
4. temperaturein refluxing ethanol for 18 h
5. customThe reaction is evaporated
6. washthe residue in ethyl acetate is washed with NaHCO3 (aqueous)
7. dry with materialdried over MgSO4
8. customevaporated