反应详情

To 259 mg (26.9 mmol) pyrimidin-5-ol (J. Chem. Soc. 1956, 2033) in 200 mL DMF are added 108 mg (26.9 mmol) sodium hydride (60% dispersion in mineral oil). The mixture is stirred for 20 min at r.t. After that time, 500 mg (22.4 mmol) 2-fluoro-4-iodopyridine are added and the mixture is stirred for 12 h at 80° C. Subsequently the mixture is poured into water and extracted with ethyl acetate (3×). The combined organic layers are washed with brine. After drying over sodium sulphate, the solvent is removed in vacuo and the residue is purified by column chromatography (silica gel; heptane/EtOAc, 100/0→40/60).

1. stirringthe mixture is stirred for 12 h at 80° C
2. extractionextracted with ethyl acetate (3×)
3. washThe combined organic layers are washed with brine
4. dry with materialAfter drying over sodium sulphate
5. customthe solvent is removed in vacuo
6. customthe residue is purified by column chromatography (silica gel; heptane/EtOAc, 100/0→40/60)