反应详情

温度

25 °C

To a solution of [4-(2,4-difluoro-5-methoxy-phenyl)-pyridin-3-yl]-methyl-amine (70 mg, 0.28 mmol) in 2.5 mL pyridine were added 3-(methylsulfonyl)-5-(trifluoromethyl)benzoic acid (example 114, intermediate a) (90 mg, 0.34 mmol) and POCl3 (2.3 mL) dropwise at 25° C. and the reaction mixture was stirred for 12 hours at 25° C. The solvent was evaporated, the residue was dissolved in EtOAc (15 ml) and washed with 2M aqueous HCl solution (5 mL) followed by saturated NaHCO3 solution (10 mL). The organic layer was dried over anhydrous Na2SO4 and evaporated. The crude product was purified by preparative HPLC (ammonium acetate/acetonitrile) to furnish the title compound as a light yellow solid (40 mg, 29%). MS (ESI): m/z=501.2 [M+H]+.

1. customThe solvent was evaporated
2. dissolutionthe residue was dissolved in EtOAc (15 ml)
3. washwashed with 2M aqueous HCl solution (5 mL)
4. dry with materialThe organic layer was dried over anhydrous Na2SO4
5. customevaporated
6. customThe crude product was purified by preparative HPLC (ammonium acetate/acetonitrile)