反応式
[NH2:1][C:2]1[CH:7]=[N:6][CH:5]=[CH:4][N:3]=1.[C:8]1([CH:14]([N+:16]#[C-:17])[CH3:15])[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[Br:18][C:19]1[S:23][C:22]([CH:24]=O)=[CH:21][CH:20]=1.Cl(O)(=O)(=O)=O.C(=O)([O-])[O-].[Na+].[Na+]>C(Cl)(Cl)Cl>[Br:18][C:19]1[S:23][C:22]([C:24]2[N:1]=[C:2]3[CH:7]=[N:6][CH:5]=[CH:4][N:3]3[C:17]=2[NH:16][CH:14]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH3:15])=[CH:21][CH:20]=1参加物
実験手順
951 mg (10.0 mmol) of 2-aminopyrazine were dissolved together with 1.31 g (10.0 mmol) of 1-phenylethylisonitrile and 1.08 ml (10.0 mmol) of 5-bromothiophene-2-carbaldehyde in chloroform (24 ml). After addition of perchloric acid (1.00 ml), the mixture was stirred at RT for 5 d. The mixture was then combined with a sat. aq. sodium carbonate solution and the phases were separated. The aqueous phase was extracted with DCM. The combined organic phases were washed with a sat. aq. sodium carbonate solution and dried over magnesium sulfate, filtered and evaporated under a vacuum. After carrying out column chromatography (EA/DCM 1:1) with the group, 831 mg (2.1 mmol, 21% of theoretical) of [2-(5-bromothiophen-2-yl)-imidazo[1,2-a]pyrazin-3-yl]-(1-phenyl-ethyl)-amine were obtained.
後処理
- customthe phases were separated
- extractionThe aqueous phase was extracted with DCM
- washThe combined organic phases were washed with a sat. aq. sodium carbonate solution
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- customevaporated under a vacuum
出典と根拠
- ORDレコード
- ord-0fe553714ad7464ba187111b5036a939
- 出典データセット
- uspto-grants-2008_09
- 特許番号
- US07420056B2
関連ノート
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