Reaktionsgleichung
Cl.[Br:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH2:6][NH2:7].[C:11](OC(=O)C)(=[O:13])[CH3:12].O.C(OCC)(=O)C>N1C=CC=CC=1>[Br:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH2:6][NH:7][C:11](=[O:13])[CH3:12]Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To a solution of 3-bromobenzylamine hydrochloride (5.20 g) in pyridine (30 ml) was added acetic anhydride (3.2 ml) at 0° C. and the mixture was stirred at room temperature for 24 h. Water and ethyl acetate were added to the reaction mixture for partitioning, and the organic layer was washed with 1N hydrochloric acid, aqueous sodium hydrogen carbonate and brine, dried (magnesium sulfate) and concentrated under reduced pressure. The residue was recrystallized from hexane-ethyl acetate to give the title compound (4.00 g) as colorless needle crystals.
Aufarbeitung
- customfor partitioning
- washthe organic layer was washed with 1N hydrochloric acid, aqueous sodium hydrogen carbonate and brine
- dry with materialdried (magnesium sulfate)
- concentrationconcentrated under reduced pressure
- customThe residue was recrystallized from hexane-ethyl acetate
Quellen und Nachweise
- ORD-Eintrag
- ord-35cf1564147845648b941737314ce4d1
- Quelldatensatz
- uspto-grants-2003_02
- Patentnummer
- US06518257B1
Verknüpfte Notizen
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