Hydrochloric Acid → 6-Aza-2-thiothymine
反応式
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]=1参加物
5
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-e0bc982c0aa54a0c8a9ab65608f93713
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09340523B2
反応ノート
読み込み中…