反应详情

5,6-Dichloro-N-hydroxy-3-pyridinecarboximidamide (3.0 g, 0.015 mol) was slurried in toluene (30 mL) and trimethylacetyl chloride (1.93 g, 0.016 mol) added. The mixture was stirred at room temperature for one hour and then heated under reflux conditions for four hours. This was then cooled and filtered through Celite, washing with additional toluene (20 mL). Evaporation of the solvent under reduced pressure and purification of the residue by chromatography over silica (0-10% ethyl acetate:hexane) gave the desired product as a white solid (2.77 g, 68%).

1. temperatureheated under reflux conditions for four hours
2. temperatureThis was then cooled
3. filtrationfiltered through Celite
4. washwashing with additional toluene (20 mL)
5. customEvaporation of the solvent
6. customunder reduced pressure and purification of the residue by chromatography over silica (0-10% ethyl acetate:hexane)