Sulfuric Acid → HCID 131730603, Verbindung
Reaktionsgleichung
[CH3:1][CH:2]1[S:13][CH2:12][C:4]2([CH:9]3[CH2:10][CH2:11][N:6]([CH2:7][CH2:8]3)[CH2:5]2)[O:3]1.[S:14](=[O:18])(=[O:17])([OH:16])[OH:15]>C1(C)C=CC=CC=1>[CH3:1][CH:2]1[S:13][CH2:12][C:4]2([CH:9]3[CH2:10][CH2:11][N:6]([CH2:7][CH2:8]3)[CH2:5]2)[O:3]1.[S:14]([O-:18])([O-:17])(=[O:16])=[O:15]Komponenten
4
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 2.5 °C
Versuchsvorschrift
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.