Reaktionsgleichung
C([O-])([O-])=O.[K+].[K+].[NH2:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2([C:19]3[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=3)[O:18][CH2:17][CH2:16][O:15]2)=[CH:10][C:9]=1[CH:26]([C:28]1[CH:33]=[CH:32][CH:31]=[C:30]([Cl:34])[CH:29]=1)[OH:27].[Br:35][CH2:36][C:37](Br)=[O:38]>C(Cl)Cl>[Br:35][CH2:36][C:37]([NH:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2([C:19]3[CH:20]=[CH:21][C:22]([Cl:25])=[CH:23][CH:24]=3)[O:18][CH2:17][CH2:16][O:15]2)=[CH:10][C:9]=1[CH:26]([C:28]1[CH:33]=[CH:32][CH:31]=[C:30]([Cl:34])[CH:29]=1)[OH:27])=[O:38]Komponenten
5
Versuchsvorschrift
K2CO3 10% (250 ml) was added to a mixture of intermediate (9) (0.072 mol) in DCM (250 ml). Then bromo-acetyl bromide (0.072 mol) was added dropwise at room temperature. The mixture was stirred at room temperature overnight. The organic layer was separated, dried (MgSO4), filtered and the solvent was evaporated till dryness. The product was used without further purification, yielding (quant.) of 2-bromo-N-[4-[2-(4-chlorophenyl)-1,3-dioxolan-2-yl]-2-[(3-chlorophenyl)hydroxymethyl]phenyl]-acetamide (intermediate 10).
Aufarbeitung
- customThe organic layer was separated
- dry with materialdried (MgSO4)
- filtrationfiltered
- customthe solvent was evaporated till dryness
- customThe product was used without further purification
Quellen und Nachweise
- ORD-Eintrag
- ord-53f0595b634948e0813ef477d7935be0
- Quelldatensatz
- uspto-grants-2006_12
- Patentnummer
- US07153958B2
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