Boron tribromide → HCID 68428755, Verbindung
Reaktionsgleichung
B(Br)(Br)Br.C[O:6][C:7]1[CH:12]=[CH:11][C:10]([N:13]2[C:17](=[O:18])[O:16][C:15]([C:19]([CH3:22])([CH3:21])[CH3:20])=[N:14]2)=[CH:9][CH:8]=1>ClCCl>[OH:6][C:7]1[CH:8]=[CH:9][C:10]([N:13]2[C:17](=[O:18])[O:16][C:15]([C:19]([CH3:22])([CH3:21])[CH3:20])=[N:14]2)=[CH:11][CH:12]=1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
3.5 g of boron tribromide are slowly added dropwise, at −60°, to a mixture of 70 ml of dichloromethane and 1.5 g of 1-methoxy-4-(5-oxo-2-tert-butyl-3,4-diaza-1-oxa-cyclopent-2-en-4-yl)-benzene. The reaction mixture is stirred at room temperature for 12 hours and then discharged onto ice/water. The aqueous mixture is extracted with dichloromethane, the extract is washed with water and concentrated and the residue is recrystallised from toluene/pentane, yielding 1-hydroxy-4-(5-oxo-2-tert-butyl-3,4-diaza-1-oxa-cyclopent-2-en-4-yl)-benzene, which melts at from 170° to 172°.
Aufarbeitung
- extractionThe aqueous mixture is extracted with dichloromethane
- washthe extract is washed with water
- concentrationconcentrated
- customthe residue is recrystallised from toluene/pentane
Quellen und Nachweise
- ORD-Eintrag
- ord-51b37236371b45218905024b8fcdf736
- Quelldatensatz
- uspto-grants-2010_05
- Patentnummer
- US07723362B2
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