Nalmefene → Nalmefene hydrochloride dihydrate
Reaktionsgleichung
[CH2:1]=[C:2]1[C@@H:15]2[O:16][C:12]3[C:13]4[C@:14]52[CH2:17][CH2:18][N:19]([CH2:20][CH:21]2[CH2:23][CH2:22]2)[C@H:6]([CH2:7][C:8]=4[CH:9]=[CH:10][C:11]=3[OH:24])[C@:5]5([OH:25])[CH2:4][CH2:3]1.[ClH:26].C=C1[C@@H]2[O:42]C3C4[C@]52CCN(CC2CC2)[C@H](CC=4C=CC=3O)[C@]5(O)CC1>>[CH2:1]=[C:2]1[C@@H:15]2[O:16][C:12]3=[C:11]([OH:24])[CH:10]=[CH:9][C:8]4=[C:13]3[C@:14]32[CH2:17][CH2:18][N:19]([CH2:20][CH:21]2[CH2:22][CH2:23]2)[C@H:6]([CH2:7]4)[C@:5]3([OH:25])[CH2:4][CH2:3]1.[OH2:42].[OH2:16].[ClH:26]Komponenten
3
Reaktionsbedingungen
- Temperatur
- 20 °C
Versuchsvorschrift
At 50° C., Nalmefene Hydrochloride was added as seeding. The seed did not dissolve and Nalmefene started to crystallize. When the cooling ramp was terminated the suspension was maintained under stirring at 20° C. for 2.5 days. The solid was filtered and washed with acetone (50 ml). The wet product was dried overnight under vacuum at 40° C. yielding 13.2 g of Nalmefene hydrochloride dihydrate (chemical purity 99.74%, water content 8.54% w/w as measured by Karl Fisher titration).