Reaktionsgleichung
[N+:1]([C:4]1[CH:9]=[C:8]([C:10]([F:13])([F:12])[F:11])[CH:7]=[CH:6][C:5]=1[OH:14])([O-:3])=[O:2].C(=O)([O-])[O-].[Ca+2].Br[C:21]([CH3:25])([CH3:24])[CH:22]=[O:23]>CN(C)C=O>[N+:1]([C:4]1[CH:9]=[C:8]([C:10]([F:11])([F:12])[F:13])[CH:7]=[CH:6][C:5]=1[O:14][C:21]([CH3:25])([CH3:24])[CH:22]=[O:23])([O-:3])=[O:2]Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To a mixture of 10 g of 2-nitro-4-trifluoromethylphenol, 8.0 g of anhydrous calcium carbonate and 30 ml of N,N-dimethylformamide was added dropwise a solution of 8.8 g of 2-bromoisobutyraldehyde in 23 ml of N,N-dimethylformamide and the mixture was stirred at room temperature for 4 days. The reaction mixture was then poured in ice-water and extracted with toluene. The organic layer was washed with 0.5 N aqueous sodium hydroxide solution and water in that order and dried over anhydrous magnesium sulfate and the solvent was distilled off. The residue was chromatographed on a silica gel column and elution was carried out with hexane-ethyl acetate (3:1). The Crystals from the eluate were recrystallized from 15 ml of hexane twice to give 4.428 g of 2-(2-nitro-4-trifluoromethylphenoxy)isobutyraldehyde.
Aufarbeitung
- extractionextracted with toluene
- washThe organic layer was washed with 0.5 N aqueous sodium hydroxide solution and water in that order
- dry with materialdried over anhydrous magnesium sulfate
- distillationthe solvent was distilled off
- customThe residue was chromatographed on a silica gel column and elution
- customThe Crystals from the eluate were recrystallized from 15 ml of hexane twice
Quellen und Nachweise
- ORD-Eintrag
- ord-90fe87addf29438a8e3aa7aa6b4f105f
- Quelldatensatz
- uspto-grants-1995_05
- Patentnummer
- US05420126
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