Reaktionsgleichung
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([OH:11])=[O:10])=[CH:4][CH:3]=1.OS(O)(=O)=O.C([O-])([O-])=O.[K+].[K+].[CH2:23](O)[CH3:24]>>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][C:9]([O:11][CH2:23][CH3:24])=[O:10])=[CH:6][CH:7]=1Komponenten
5
Versuchsvorschrift
A solution of 43 g (200 mmol) of 4-bromophenylacetic acid and 0.2 g of conc. H2SO4 in 470 ml of ethanol was refluxed for 16 hours. The reaction mixture was cooled to ambient temperature, stirred with 6 g of solid K2CO3 for 30 minutes and then filtered. The filtrate was concentrated in vacuo, diluted with Et2O (200 ml), washed with 10% aqueous NaHCO3 (10 ml) and brine (10 ml), dried over MgSO4 and concentrated in vacuo to give the title compound as a colorless oil.
Aufarbeitung
- filtrationfiltered
- concentrationThe filtrate was concentrated in vacuo
- additiondiluted with Et2O (200 ml)
- washwashed with 10% aqueous NaHCO3 (10 ml) and brine (10 ml)
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-af99be4195cf4b468b417da2a68b4f2e
- Quelldatensatz
- uspto-grants-2005_02
- Patentnummer
- US06855832B2
Verknüpfte Notizen
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