Cesium carbonate → HCID 136304034、化合物
反応式
[O:1]=[C:2]1[N:7]2[CH:8]=[C:9]([C:11]([O:13]CC)=[O:12])[N:10]=[C:6]2[CH:5]=[CH:4][NH:3]1.C(=O)([O-])[O-].[Cs+].[Cs+]>C(O)C.O>[O:1]=[C:2]1[N:7]2[CH:8]=[C:9]([C:11]([OH:13])=[O:12])[N:10]=[C:6]2[CH:5]=[CH:4][NH:3]1参加物
5
実験手順
Ethyl 5-oxo-5,6-dihydroimidazo[1,2-c]pyrimidine-2-carboxylate (2.510 mmol, 0.52 g) was suspended in ethanol (20 ml). Cesium carbonate (5.02 mmol, 1.635 g) dissolved in water (4 ml) was added and the resulting mixture was stirred at RT for 3.5 h after which the mixture was refluxed for 8 h. The ethanol was evaporated, and the residue was diluted with water. The pH was adjusted to 4 with 1 M HCl and the solvent was evaporated. The residue was purified by trituration from DMF. 0.137 g of the title compound was obtained. 1H-NMR (400 MHz, CDCl3): δ 7.17-7.31 (m, 2H), 7.86-7.99 (m, 1H).
後処理
- additionwas added
- temperaturewas refluxed for 8 h
- customThe ethanol was evaporated
- additionthe residue was diluted with water
- customthe solvent was evaporated
- customThe residue was purified by trituration from DMF
出典と根拠
- ORDレコード
- ord-05957157090a46ac96547bc412afa171
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08921378B2
反応ノート
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