反応式
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([O:11][CH2:12][CH2:13][CH2:14][Cl:15])=[CH:7][C:6]=1[F:16])=O.[NH2:17][C:18]1[CH:23]=[C:22]([CH3:24])[CH:21]=[CH:20][N:19]=1>C(O)C>[Cl:15][CH2:14][CH2:13][CH2:12][O:11][C:8]1[CH:9]=[CH:10][C:5]([C:3]2[N:17]=[C:18]3[CH:23]=[C:22]([CH3:24])[CH:21]=[CH:20][N:19]3[CH:2]=2)=[C:6]([F:16])[CH:7]=1参加物
4
実験手順
A solution of the product of Step B (1.0 g) and 2-amino-4-picoline (0.357 g) in ethanol (4 mL) was heated at 73° C. for 18 hours. The reaction mixture was cooled to ambient temperature and the solvent evaporated in vacuo. A portion of the residue was purified via silica gel chromatography (ethyl acetate/hexane) directly. The remainder of the residue was dissolved in methanol/dichloromethane and treated with Dowex® 550A basic resin (Aldrich, Milwaukee, Wis.) for 10 minutes. The resin was removed via filtration and the filtrate evaporated prior to silica gel chromatography (ethyl acetate/hexane). The combined material (0.42 g) containing the title compound was used without further purification.
後処理
- customthe solvent evaporated in vacuo
- customA portion of the residue was purified via silica gel chromatography (ethyl acetate/hexane) directly
- dissolutionThe remainder of the residue was dissolved in methanol/dichloromethane
- additiontreated with Dowex® 550A basic resin (Aldrich, Milwaukee, Wis.) for 10 minutes
- customThe resin was removed via filtration
- customthe filtrate evaporated
- additionThe combined material (0.42 g) containing the title compound
- customwas used without further purification
出典と根拠
- ORDレコード
- ord-95e42f03238643bf8dd17789479a8a05
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07087757B2
関連ノート
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