FV-100 free base → HCID 56962118, Verbindung
Reaktionsgleichung
[NH2:1][C@@H:2]([CH:34]([CH3:36])[CH3:35])[C:3]([O:5][CH2:6][C@@H:7]1[C@@H:11]([OH:12])[CH2:10][C@H:9]([N:13]2[CH:18]=[C:17]3[CH:19]=[C:20]([C:22]4[CH:27]=[CH:26][C:25]([CH2:28][CH2:29][CH2:30][CH2:31][CH3:32])=[CH:24][CH:23]=4)[O:21][C:16]3=[N:15][C:14]2=[O:33])[O:8]1)=[O:4].[ClH:37].CC(O)C>>[ClH:37].[NH2:1][CH:2]([CH:34]([CH3:35])[CH3:36])[C:3]([O:5][CH2:6][C@@H:7]1[C@@H:11]([OH:12])[CH2:10][C@H:9]([N:13]2[CH:18]=[C:17]3[CH:19]=[C:20]([C:22]4[CH:23]=[CH:24][C:25]([CH2:28][CH2:29][CH2:30][CH2:31][CH3:32])=[CH:26][CH:27]=4)[O:21][C:16]3=[N:15][C:14]2=[O:33])[O:8]1)=[O:4]Komponenten
3
Versuchsvorschrift
The above reaction mixture from Example 15 was cooled below 5° C. and was added with 20% of HCl IPA solution until pH 1˜4. The mixture was stirred for additional 1 h and was filtered. The filter cake was washed with 34.6 kg of dichloromethane. Desired crude product was obtained. The overall yield from Example 12 was 67% and the purity was 97%. The crude product was recrystallized with methanol/dichloromethane/MTBE to give the desired pure product.
Aufarbeitung
- temperaturewas cooled below 5° C.
- filtrationwas filtered
- washThe filter cake was washed with 34.6 kg of dichloromethane