Dimethylformamide → 7-Chlorothieno[3,2-b]pyridine-2-carboxamide
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]2[CH:8]=[C:9]([C:11]([O-:13])=O)[S:10][C:3]=12.[Li+].S(Cl)(Cl)=O.C(Cl)Cl.C[N:23](C=O)C>>[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]2[CH:8]=[C:9]([C:11]([NH2:23])=[O:13])[S:10][C:3]=12参加物
5
実験手順
A solution of lithium 7-chloro-thieno[3,2-b]pyridine-2-carboxylate (1.0 g, 4.7 mmol), thionyl chloride (7.0 mmol, 3.5 mL), CH2Cl2 (40 mL), and DMF (0.4 mL) was heated to reflux. After 3 h the resulting yellow solution was concentrated under reduced pressure, the resulting residue was suspended in CH2Cl2 (60 mL), and NH3 gas was bubbled through the mixture for 10 min. The reaction mixture was filtered to give the title compound as a white solid (1.17 g, 100%). MS: 213.0/215.1 (MH+); HPLC Rf: 3.44 min; HPLC purity: 98%.
後処理
- concentrationAfter 3 h the resulting yellow solution was concentrated under reduced pressure
- customNH3 gas was bubbled through the mixture for 10 min
- filtrationThe reaction mixture was filtered
出典と根拠
- ORDレコード
- ord-3763133b7c0a4b97a245ec79a573e7dd
- 出典データセット
- uspto-grants-2005_11
- 特許番号
- US06964961B2
反応ノート
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