Reaktionsgleichung
C(O)(=O)C(O)=O.C([N:14]1[CH2:19][CH2:18][CH:17]([CH2:20][NH:21][C:22]([C:24]2[C:32]3[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=3[N:26]3[CH2:33][CH2:34][CH2:35][O:36][C:25]=23)=[O:23])[CH2:16][CH2:15]1)C1C=CC=CC=1>C(O)C.C(O)(=O)C.[Pd]>[NH:14]1[CH2:19][CH2:18][CH:17]([CH2:20][NH:21][C:22]([C:24]2[C:32]3[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=3[N:26]3[CH2:33][CH2:34][CH2:35][O:36][C:25]=23)=[O:23])[CH2:16][CH2:15]1Komponenten
Edukt 1
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 3
Versuchsvorschrift
A stirred suspension of N-[(1-benzyl-4-piperidyl)methyl] 3,4-dihydro-2H-[1,3]oxazino[3,2-a]indole-10-carboxamide oxalate salt (E20, 2.25 g, 0.0046 mole) in ethanol (100 ml) and glacial acetic acid (4 ml) was hydrogenated over 10% Pd-C (0.8 g) at atmospheric pressure and 45° C. for 18 h. The mixture was filtered and the filtrate concentrated in vacuo. The majority of the product was in the solid which had been filtered off. This material was shaken with concentrated potassium carbonate solution (50 ml) and chloroform (50 ml) together with the residue from the filtrate. The mixture was filtered, the chloroform layer separated and dried (Na2SO4), then concentrated in vacuo to afford the title compound as a white solid (1.52 g, 100%). This was recrystallised from chlorofornm/60-80 petrol mp 139-141° C.
Aufarbeitung
- filtrationThe mixture was filtered
- concentrationthe filtrate concentrated in vacuo
- filtrationhad been filtered off
- filtrationThe mixture was filtered
- customthe chloroform layer separated
- dry with materialdried (Na2SO4)
- concentrationconcentrated in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-ed20c27d31994e61b67e037e60ae3473
- Quelldatensatz
- uspto-grants-1999_12
- Patentnummer
- US05998409
Verknüpfte Notizen
Wird geladen…