Phosphorus oxychloride → 7-Chloro-3-methylthieno(3,2-b)pyridine
反応式
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]=12参加物
4
実験手順
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%).
後処理
- temperatureat reflux under nitrogen
- temperaturecooled
- concentrationconcentrated
- additionSaturated NaHCO3 solution was carefully added
- extractionThe biphasic mixture was extracted with dichloromethane
- customdried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-442ece535ad7424db7116af6e8149339
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08022223B2
反応ノート
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