Reaktionsgleichung
[Cl-].[Al+3].[Cl-].[Cl-].[C:5]([N:8]1[CH2:16][CH2:15][CH:11]([C:12](Cl)=[O:13])[CH2:10][CH2:9]1)(=[O:7])[CH3:6].[F:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>>[C:5]([N:8]1[CH2:16][CH2:15][CH:11]([C:12](=[O:13])[C:21]2[CH:22]=[CH:23][C:18]([F:17])=[CH:19][CH:20]=2)[CH2:10][CH2:9]1)(=[O:7])[CH3:6]Komponenten
Versuchsvorschrift
The title compound was prepared as disclosed in U.S. Pat. No. 3,576,810 as follows: A mixture of 93 g (0.7 mole) of aluminum chloride in 150 ml of fluorobenzene was stirred while 70 g (0.37 mole) of 1-acetylisonipecotic acid chloride was added in small portions. After the addition was complete, the mixture was refluxed for one hour. The mixture was poured onto ice and the two resulting layers were separated. The aqueous layer was extracted twice with chloroform and the chloroform extracts were added to the fluorobenzene which was separated previously. The organic solution was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated and 73.7 g (80%) of 1-acetyl-4-(p-fluorobenzoyl)-piperidine was obtained as a crystalline residue. Recrystallization from ligroin-isopropyl ether gave a white crystalline product melting at 75°-78° C.
Aufarbeitung
- customThe title compound was prepared
- additionwas added in small portions
- additionAfter the addition
- temperaturethe mixture was refluxed for one hour
- additionThe mixture was poured onto ice
- customthe two resulting layers were separated
- extractionThe aqueous layer was extracted twice with chloroform
- additionthe chloroform extracts were added to the fluorobenzene which
- customwas separated previously
- dry with materialThe organic solution was dried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationThe filtrate was concentrated
Quellen und Nachweise
- ORD-Eintrag
- ord-79ff20058e874daeb6a8df84bce5fc68
- Quelldatensatz
- uspto-grants-1989_12
- Patentnummer
- US04886794
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