2-Aminothiophene-3-carboxamide → 2-sulfanyl-3H,4H-thieno(2,3-d)pyrimidin-4-one
反応式
[NH2:1][C:2]1[S:3][CH:4]=[CH:5][C:6]=1[C:7]([NH2:9])=[O:8].C(O[C:13]([S-])=[S:14])C.[K+]>CN(C=O)C>[S:14]=[C:13]1[NH:1][C:2]2[S:3][CH:4]=[CH:5][C:6]=2[C:7](=[O:8])[NH:9]1参加物
4
反応条件
- 温度
- 150 °C
実験手順
2-Aminothiophene-3-carboxamide (13 g, 92 mmol) and potassium ethylxanthate (48 g, 275 mmol) were mixed together and added to DMF (300 mL). The resulting mixture was heated to 150° C. for 6 hrs, then cooled to RT and concentrated on the rotovap under reduced pressure at 90° C. The residue was diluted with 300 mL of aqueous citric acid (5%) and cooled to 0° C. and stirred for 30 min. The tan powder was filtered and dried overnight to give (11.5 g) of the title compound MS (ES+): 185 (M+H)+.
後処理
- temperaturecooled to RT
- concentrationconcentrated on the rotovap under reduced pressure at 90° C
- additionThe residue was diluted with 300 mL of aqueous citric acid (5%)
- temperaturecooled to 0° C.
- filtrationThe tan powder was filtered
- customdried overnight
出典と根拠
- ORDレコード
- ord-5d20b758be07431cab5abca7aaf31268
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07745449B2
反応ノート
読み込み中…