Reaktionsgleichung
[CH3:1][C:2]1[O:3][C:4]([CH3:11])=[CH:5][C:6]=1[C:7]([O:9][CH3:10])=[O:8].OC1[CH2:18][C:17]([CH3:20])([CH3:19])[NH:16][C:15]([CH3:22])([CH3:21])[CH2:14]1>CCCCO.CCCCO.CCCCO.CCCCO.[Ti].CO>[CH3:1][C:2]1[O:3][C:4]([CH3:11])=[CH:5][C:6]=1[C:7]([O:9][CH:10]1[CH2:18][C:17]([CH3:20])([CH3:19])[NH:16][C:15]([CH3:22])([CH3:21])[CH2:14]1)=[O:8]Komponenten
5
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
154 g (1 mole) of methyl 2,5-dimethylfuran-3-carboxylate and 157 g (1 mole) of 4-hydroxy-2,2,6,6-tetramethylpiperidine were heated together with 10 g of tetrabutyl orthotitanate for 10 hours at about 190° C., the methanol formed being distilled off. When the reaction is complete, the mixture is cooled and the reaction mass is dissolved in ethyl acetate. The solution is extracted by shaking, first with 10% strength sodium carbonate solution and then with water, after which it is dried and evaporated down, and the residue is distilled under reduced pressure. The desired product distils at 142° C./2 mm as a virtually colorless oil which soon solidifies to a solid of melting point 59°-61° C.
Aufarbeitung
- distillationbeing distilled off
- temperaturethe mixture is cooled
- dissolutionthe reaction mass is dissolved in ethyl acetate
- extractionThe solution is extracted
- dry with materialwith water, after which it is dried
- customevaporated down
- distillationthe residue is distilled under reduced pressure
- customThe desired product distils at 142° C./2 mm as a virtually colorless oil which
Quellen und Nachweise
- ORD-Eintrag
- ord-66b19aa7576741619657092ed9d7f36e
- Quelldatensatz
- uspto-grants-1986_07
- Patentnummer
- US04603205
Verknüpfte Notizen
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