Hydrochloric Acid → HCID 19874067, Verbindung
Reaktionsgleichung
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=2)=[CH:4][CH:3]=1.C([O-])=O.[NH4+:21].[ClH:22].[OH-].[Na+]>>[ClH:22].[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([NH2:21])[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=2)=[CH:4][CH:3]=1Komponenten
Reaktionsbedingungen
- Temperatur
- 190 °C
Versuchsvorschrift
A mixture of 1,2-bis(4-fluorophenyl)-1-oxoethane (2.13 g) and ammonium formate (3.78 g) was stirred for 10 hours at 190° C.. After cooling, concentrated hydrochloric acid (12 ml) was added to the reaction mixture and the mixture was refluxed for 5 hours. After cooling, aqueous sodium hydroxide solution was added to the mixture and alkalized. The product was extracted with ethyl acetate and the organic layer was washed with saturated sodium chloride solution. The organic layer was dried over anhydrous magnesium sulfate and concentrated in vacuo. The oily residue was dissolved in methanol. To the solution, HCl/methanol was added and the solution was concentrated in vacuo. Separated crystals were collected by filtration to give 1.77 g (65.6%) of the titled compound.
Aufarbeitung
- temperatureAfter cooling
- temperaturethe mixture was refluxed for 5 hours
- temperatureAfter cooling
- extractionThe product was extracted with ethyl acetate
- washthe organic layer was washed with saturated sodium chloride solution
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- concentrationconcentrated in vacuo
- dissolutionThe oily residue was dissolved in methanol
- additionTo the solution, HCl/methanol was added
- concentrationthe solution was concentrated in vacuo
- customSeparated crystals
- filtrationwere collected by filtration
Quellen und Nachweise
- ORD-Eintrag
- ord-36240fb79e9e4bd69f5e81dff48ac5a8
- Quelldatensatz
- uspto-grants-1992_02
- Patentnummer
- US05087627
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