反応式
[C:1]([O:5][C:6](=[O:14])[NH:7][CH:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2].[Cl:15][C:16]1[C:21]([C:22]([F:25])([F:24])[F:23])=[CH:20][CH:19]=[C:18](Cl)[N:17]=1.C(=O)([O-])[O-].[Cs+].[Cs+].O>O1CCOCC1.C(Cl)Cl>[C:1]([O:5][C:6](=[O:14])[NH:7][CH:8]1[CH2:13][CH2:12][N:11]([C:18]2[CH:19]=[CH:20][C:21]([C:22]([F:24])([F:25])[F:23])=[C:16]([Cl:15])[N:17]=2)[CH2:10][CH2:9]1)([CH3:4])([CH3:2])[CH3:3]参加物
7
実験手順
A stirred mixture of D7 (5.0 g, 25 mmol), 2,6-dichloro-3-trifluoromethyl-pyridine (5.4 g, 25 mmol) and cesium carbonate (12.22 g, 37.5 mmol) in 1,4-dioxane (75 mL) was heated at reflux under argon for 64 h. To the mixture, which was cooled to ambient temperature, was added water (250 mL) and DCM (250 mL) with shaking and the layers were separated. The aqueous phase was further extracted with DCM (250 mL) and the combined organic extracts were dried (MgSO4) and evaporated in vacuo to an oil. This material was purified by chromatography over silica gel eluting with a gradient of ethyl acetate/hexane to afford the title compounds
後処理
- temperaturewas heated
- temperatureat reflux under argon for 64 h
- customthe layers were separated
- extractionThe aqueous phase was further extracted with DCM (250 mL)
- dry with materialthe combined organic extracts were dried (MgSO4)
- customevaporated in vacuo to an oil
- customThis material was purified by chromatography over silica gel eluting with a gradient of ethyl acetate/hexane
出典と根拠
- ORDレコード
- ord-25b85cbeb7de498898bbe3ec1d392877
- 出典データセット
- uspto-grants-2009_05
- 特許番号
- US07528151B2
関連ノート
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