Hydrochloric Acid → 6-Aza-2-thiothymine
Reaktionsgleichung
C([O-])([O-])=O.[Na+].[Na+].[C:7]([NH:10][N:11]=[C:12]([CH3:16])[C:13](O)=[O:14])(=[S:9])[NH2:8].Cl>O>[CH3:16][C:12]1[C:13](=[O:14])[NH:8][C:7](=[S:9])[NH:10][N:11]=1Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To a solution of Na2CO3 (4.84 g, 45.6 mmol) in water (300 mL) was added 2-(2-carbamothioylhydrazono)propanoic acid (3, 7.35 g, 45.6 mmol). The mixture was heated at refluxing temperature for 3.5 h. After cooling to room temperature, the clear solution was acidified with 2 N HCl to pH˜5. The mixture was extracted with EtOAc (60 mL×4) and CH2Cl2 (60 mL×4). The combined extracts were dried over Na2SO4 and concentrated to give 6-methyl-3-thioxo-3,4-dihydro-1,2,4-triazin-5(2H)-one (4) as a white solid. MS: m/z, 144 (100%, M+1).
Aufarbeitung
- temperatureThe mixture was heated
- temperatureat refluxing temperature for 3.5 h
- extractionThe mixture was extracted with EtOAc (60 mL×4) and CH2Cl2 (60 mL×4)
- dry with materialThe combined extracts were dried over Na2SO4
- concentrationconcentrated
Quellen und Nachweise
- ORD-Eintrag
- ord-e0bc982c0aa54a0c8a9ab65608f93713
- Quelldatensatz
- uspto-grants-2016_05
- Patentnummer
- US09340523B2
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