Potassium Carbonate → 5-bromothieno[2,3-b]pyridine
반응식
[Br:1][C:2]1[CH:3]=[C:4]2[CH:10]=[C:9]([Si](C)(C)C)[S:8][C:5]2=[N:6][CH:7]=1.C([O-])([O-])=O.[K+].[K+]>C(O)C>[Br:1][C:2]1[CH:3]=[C:4]2[CH:10]=[CH:9][S:8][C:5]2=[N:6][CH:7]=1참가 물질
4
반응 조건
- 온도
- 65 °C
실험 절차
The 5-bromo-2-(trimethylsilyl)thieno[2,3-b]pyridine from Part A (8.99 g, 31.4 mmol) was dissolved in ethanol (70 mL), followed by addition of K2CO3 (10.85 g, 78.5 mmol). Reaction was stirred at 65° C. for 1 hour. The reaction mixture was allowed to cool to 25° C., concentrated to dryness, and dissolved in EtOAc (150 mL). The solution was washed with H2O (80 mL), and brine (150 mL), dried over Na2SO4, filtered, and concentrated to yield white solid, 5-bromothieno[2,3-b]pyridine, 6.57 g (98%). 1H NMR (300 MHz, CDCl3) δ 8.60 (d, J≦2.2 Hz, 1H), 8.16 (d, J=2.2 Hz 1H), 7.57 (d, J=6.0 Hz 1H), 7.21 (d, J=6.0 Hz, 1H).
후처리
- customReaction
- temperatureto cool to 25° C.
- concentrationconcentrated to dryness
- dissolutiondissolved in EtOAc (150 mL)
- washThe solution was washed with H2O (80 mL), and brine (150 mL)
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-6fc6a89b83e442d4b3ce603f2118a6fa
- 출처 데이터셋
- uspto-grants-2013_11
- 특허 번호
- US08591943B2
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