反应详情

To a mixture of 10.0 g of 2-mercapto-3-pyridinol, 11.0 g of potassium carbonate and 100 mL of 2-butanone was added dropwise with stirring, 13.3 g of benzyl bromide. After stirring at 22° C. for two hours, the mixture was heated to reflux for thirty minutes. The reaction mixture was concentrated under reduced pressure, the residue treated with water, and the mixture brought to pH 6 by the addition of acetic acid. The crude product was filtered and recrystallized from toluene to give 11.1 g of the title compound as a grey crystalline solid, mp 103–104° C. The structure of the product was confirmed by its 1H nmr and mass spectra.

1. additionwas added dropwise
2. stirringAfter stirring at 22° C. for two hours
3. temperaturethe mixture was heated
4. temperatureto reflux for thirty minutes
5. concentrationThe reaction mixture was concentrated under reduced pressure
6. additionthe residue treated with water
7. additionthe mixture brought to pH 6 by the addition of acetic acid
8. filtrationThe crude product was filtered
9. customrecrystallized from toluene