Phosphorus oxychloride → 7-Chloro-3-methylthieno(3,2-b)pyridine
반응식
P(Cl)(Cl)([Cl:3])=O.[CH3:6][C:7]1[C:11]2=[N:12][CH:13]=[CH:14][C:15](O)=[C:10]2[S:9][CH:8]=1>ClCCCl>[Cl:3][C:15]1[CH:14]=[CH:13][N:12]=[C:11]2[C:7]([CH3:6])=[CH:8][S:9][C:10]=12참가 물질
4
실험 절차
Phosphorous oxychloride (2.2 mL, 24 mmol) in 1,2-dichloroethane (12 mL) was charged with 3-methylthieno[3,2-b]pyridin-7-ol (2.0 g, 12 mmol). The reaction stirred overnight at reflux under nitrogen. The mixture was the cooled and concentrated. Saturated NaHCO3 solution was carefully added to neutralize the residue. The biphasic mixture was extracted with dichloromethane, dried, and concentrated. Flash chromatography (15% EtOAc/hexanes) gave the title compound (1.23 g, 55%).
후처리
- temperatureat reflux under nitrogen
- temperaturecooled
- concentrationconcentrated
- additionSaturated NaHCO3 solution was carefully added
- extractionThe biphasic mixture was extracted with dichloromethane
- customdried
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-442ece535ad7424db7116af6e8149339
- 출처 데이터셋
- uspto-grants-2011_09
- 특허 번호
- US08022223B2
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