Dimethylformamide → 7-Chlorothieno[3,2-b]pyridine-2-carboxamide
반응식
[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]=12참가 물질
5
실험 절차
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%.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-3763133b7c0a4b97a245ec79a573e7dd
- 출처 데이터셋
- uspto-grants-2005_11
- 특허 번호
- US06964961B2
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