反应详情

21.5 g (156 mmol) of potassium carbonate was added to a suspension of 29.4 g (120 mmol) of 1,4-dihydro-5-(phenylmethoxy)-4-oxo-2-pyridinecarboxylic acid in 350 ml of N,N-dimethylformamide (DMF) and stirred for 1 hour at room temperature. 31 ml (264 mmol) of benzylbromide was added and the mixture was heated at 100° C. under stirring for 25 hours. After cooling to room temperature, the DMF was distilled off in vacuo and the residue triturated with ethyl acetate with short heating to 60° C. 40 g of inorganic salts were filtered off, the filtrate was concentrated to ca. 75 ml and chromatographed on silica gel with ethyl acetate:petroleum ether 90:10 as eluent. Yield: 35.5 g; melting point 116.7° C.

1. temperaturethe mixture was heated at 100° C.
2. stirringunder stirring for 25 hours
3. temperatureAfter cooling to room temperature
4. distillationthe DMF was distilled off in vacuo
5. customthe residue triturated with ethyl acetate
6. temperaturewith short heating to 60° C
7. filtration40 g of inorganic salts were filtered off
8. concentrationthe filtrate was concentrated to ca. 75 ml
9. customchromatographed on silica gel with ethyl acetate:petroleum ether 90:10 as eluent