Potassium Carbonate → Ethyl 5-(2,2-difluoroethoxy)-3-fluoro-pyridine-2-carboxylate

反応式

[F:1][C:2]1[C:3]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[N:4][CH:5]=[C:6](F)[CH:7]=1.[F:14][C:15]([F:18])(O)[CH3:16].C(=O)([O-])[O-:20].[K+].[K+]>C(#N)C>[F:14][CH:15]([F:18])[CH2:16][O:20][C:6]1[CH:7]=[C:2]([F:1])[C:3]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[N:4][CH:5]=1

参加物

実験手順

Ethyl 3,5-difluoropyridine-2-carboxylate (0.98 g, 5.24 mmol) is dissolved in acetonitrile (20 mL). Difluoroethanol (430 μL, 6.81 mmol) is added followed by potassium carbonate (1.83 g, 13.09 mmol). The solution is stirred at room temperature for 2 days then filtered and the filtrate is concentrated. The crude material is purified via silica gel chromatography eluting with a 0-25-50% ethyl acetate/hexanes gradient to give the title compound (242 mg, 18%). ES/MS (m/e): 250.0 (M+1).