Hydrogen Peroxide → HCID 178431782, Verbindung
Reaktionsgleichung
OO.[CH:3]([C:6]1[NH:11][C:10](=S)[NH:9][C:8](=[O:13])[C:7]=1[CH3:14])([CH3:5])[CH3:4].C(=O)([O-])[O-].[Na+].[Na+].S([O-])([O-])(=O)=S.[Na+].[Na+]>O>[CH:3]([C:6]1[N:11]=[CH:10][N:9]=[C:8]([OH:13])[C:7]=1[CH3:14])([CH3:5])[CH3:4]Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 70 °C
Versuchsvorschrift
To a solution of 30% hydrogen peroxide (12 mL) and water (23 mL) was slowly added 6-isopropyl-5-methyl-2-thioxo-2,3-dihydropyrimidin-4(1H)-one (1.0 g, 5.4 mmol). The reaction mixture was stirred at 70° C. for 3 h. After cooling to room temperature, saturated sodium carbonate was slowly added until the pH reached 10. To this mixture was slowly added a 1 M solution of sodium thiosulfate until residual peroxide was quenched, whereupon the aqueous solution was concentrated to dryness. The residue was suspended in chloroform (100 mL), filtered to remove inorganic salts and the filtrate concentrated to provide 6-isopropyl-5-methylpyrimidin-4-ol (0.25 g, 30% yield) as a white solid that was used without further purification. MS (EI) for C8H12N2O: 153 (MH+).
Aufarbeitung
- temperatureAfter cooling to room temperature
- customwas quenched, whereupon the aqueous solution
- concentrationwas concentrated to dryness
- filtrationfiltered
- customto remove inorganic salts
- concentrationthe filtrate concentrated
Quellen und Nachweise
- ORD-Eintrag
- ord-0ca1d605bdbf4a15acb0c366a0bc203b
- Quelldatensatz
- uspto-grants-2014_02
- Patentnummer
- US08648066B2
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