Methanesulfonic Acid → Lurosetron Mesylate
Reaktionsgleichung
[F:1][C:2]1[C:10]2[N:9]([CH3:11])[C:8]3[CH2:12][CH2:13][N:14]([CH2:17][C:18]4[N:19]=[CH:20][NH:21][C:22]=4[CH3:23])[C:15](=[O:16])[C:7]=3[C:6]=2[CH:5]=[CH:4][CH:3]=1.[CH3:24][S:25]([OH:28])(=[O:27])=[O:26]>>[CH3:24][S:25]([OH:28])(=[O:27])=[O:26].[F:1][C:2]1[C:10]2[N:9]([CH3:11])[C:8]3[CH2:12][CH2:13][N:14]([CH2:17][C:18]4[N:19]=[CH:20][NH:21][C:22]=4[CH3:23])[C:15](=[O:16])[C:7]=3[C:6]=2[CH:5]=[CH:4][CH:3]=1Komponenten
3
Reaktionsbedingungen
- Temperatur
- 4 °C
Versuchsvorschrift
6-Fluoro-2,3,4,5-tetrahydro-5-methyl-2-[(5-methyl-1H-imidazol-4-yl)methyl]-1H-pyrido[4,3-b]indol-1-one (224.9 g) was suspended in IMS (1125 ml) and heated to reflux. A solution of methanesulphonic acid (69.2 g) in IMS (675 ml) was added with stirring over 15 minutes. The mixture was subsequently allowed to cool over 3 hours, then seeded and left overnight at ambient temperature before being cooled to 4° C. for 5 hours, with stirring. The mixture was filtered, the solid washed with cold IMS (2×450 ml), and then dried between 40° and 76° C. in vacuo to give the title compound (226 g) as a crystalline solid.