反应详情

温度

2.5 °C

Charged toluene (50 ml) and to this charged cevimeline free base with cis isomer >90% (5.0 g) (prepared by any one of the above methods given in examples III to V). Stirred for 10 to 15 minutes to obtain a clear solution. Cooled the solution to 0 to 5° C. Charged concentrated sulfuric acid (1.3 ml) drop wise over 30 minutes and stir the resultant liberated sulfate salt for 30 minutes at 0 to 5° C. Then slowly raised the temperature to reflux temperature (100 to 115° C.) and continued the reflux for 60 to 90 minutes. The reaction mass was then cooled and processed as in Example VI to yield 3.5 g of cevimeline sulfate with cis isomer >97% purity by HPLC.

1. customto obtain a clear solution
2. stirringstir the resultant
3. customfor 30 minutes
4. customat 0 to 5° C
5. temperatureThen slowly raised the temperature
6. temperatureto reflux temperature (100 to 115° C.)
7. temperaturereflux for 60 to 90 minutes
8. temperatureThe reaction mass was then cooled