Reaktionsgleichung
F[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9].[CH2:11]([O:13][C:14]([C:16]1[N:17]=[CH:18][NH:19][C:20]=1[C:21]([O:23][CH2:24][CH3:25])=[O:22])=[O:15])[CH3:12].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH2:24]([O:23][C:21]([C:20]1[N:19]=[CH:18][N:17]([C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=2[N+:8]([O-:10])=[O:9])[C:16]=1[C:14]([O:13][CH2:11][CH3:12])=[O:15])=[O:22])[CH3:25]Komponenten
5
Versuchsvorschrift
To a solution of o-fluoronitrobenzene (106 g) and imidazole 4,5-dicarboxylic acid diethyl ester (106 g) in one liter of N,N-dimethyl formamide (DMF) was added anhydrous potassium carbonate (200 g). The reaction mixture was stirred vigorously for at least four hours. After removal of solvent under oil pump vacuum, the residue was treated with water, then extracted with chloroform (300 ml×3). The combined chloroform extracts were washed with water, dried by magnesium sulfate, then concentrated under vacuum to an oil. Upon treatment with ether, the oil was solidified and the product was obtained as a white solid (136 g, 81% yield). Recrystallized from chloroform-hexane, m.p. 93°-95° C.
Aufarbeitung
- customAfter removal of solvent under oil pump vacuum
- additionthe residue was treated with water
- extractionextracted with chloroform (300 ml×3)
- washThe combined chloroform extracts were washed with water
- dry with materialdried by magnesium sulfate
- concentrationconcentrated under vacuum to an oil
Quellen und Nachweise
- ORD-Eintrag
- ord-b1eac2400ee844e2a7b3c94ea815c4bf
- Quelldatensatz
- uspto-grants-1984_04
- Patentnummer
- US04440929
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