Reaktionsgleichung
[CH3:1][NH:2][C:3]([NH2:5])=[O:4].O1CCCC1.[C:11](Cl)(=[O:15])[C:12](Cl)=[O:13].C(OCC)(=O)C>O>[CH3:1][N:2]1[C:12](=[O:13])[C:11](=[O:15])[NH:5][C:3]1=[O:4]Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
6.6 g of methylurea was added to 200 ml of anhydrous tetrahydrofuran and the suspension was stirred in an ice-water bath. 12.5 g of oxalyl chloride was added dropwise to the suspension, and the stirring was continued for 30 minutes in an ice-water bath. 200 ml of ethyl acetate and 70 ml of water were added to the reaction mixture and the organic layer was obtained by extraction. The water layer was further extracted with 130 ml of ethyl acetate. The resulting organic layer was dried over anhydrous sodium sulfate and evaporated to dryness, and the crude residue was recrystallized from ethyl acetate-hexane to give 10.0 g of 1-methylimidazolidinetrione in the form of colorless needle crystals. The resulting compound was stirred in 1N ammonia water for a hour at room temperature. The solution was evaporated to dryness and the residue was recrystallized from water-ethanol to give 7.7 g of 5-methyloxaluric acid ammonium salt (compound 1) in the form of colorless prism crystals.
Aufarbeitung
- customthe organic layer was obtained by extraction
- extractionThe water layer was further extracted with 130 ml of ethyl acetate
- dry with materialThe resulting organic layer was dried over anhydrous sodium sulfate
- customevaporated to dryness
- customthe crude residue was recrystallized from ethyl acetate-hexane
Quellen und Nachweise
- ORD-Eintrag
- ord-5ed321ce7c8e41d2aee810344d8b8561
- Quelldatensatz
- uspto-grants-1987_11
- Patentnummer
- US04708954
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