反应详情

温度

-50 °C

To a solution of 7.1 g (0.026 moles) of procainamide hydrochloride in 100 ml acetone and 5 ml triethylamino at -50° C., is added slowly 5.0 g (0.026 moles) of α-toluenesulfonyl chloride. Stir at -50° C. for 1 hour, then warm to room temperature and stir for 16 hours. Remove the solvent in vacuo. Slurry the residue in 200 ml ether, and wash 2×100 ml portions of methylene chloride. The combined methylene chloride extracted are vacuum stripped to dryness. The residue is dissolved in 100 ml ethanol and brought to pH 3 with concentrated hydrochloric acid. The solvent is removed in vacuo, and the residue triturated with methylene-chloride to provide the title compound.

1. temperaturewarm to room temperature
2. stirringstir for 16 hours
3. customRemove the solvent in vacuo
4. washwash 2×100 ml portions of methylene chloride
5. extractionThe combined methylene chloride extracted
6. dissolutionThe residue is dissolved in 100 ml ethanol
7. customThe solvent is removed in vacuo
8. customthe residue triturated with methylene-chloride