反応式
Cl.[N:2]1[CH:7]=[CH:6][CH:5]=[C:4]([S:8](Cl)(=[O:10])=[O:9])[CH:3]=1.[NH2:12][C:13]1[CH:14]=[C:15]([C@@H:19]([NH:21][C:22]2[CH:27]=[N:26][CH:25]=[C:24]([Cl:28])[N:23]=2)[CH3:20])[CH:16]=[CH:17][CH:18]=1.C(N(CC)CC)C>ClCCl.C(OCC)(=O)C>[Cl:28][C:24]1[N:23]=[C:22]([NH:21][C@H:19]([C:15]2[CH:14]=[C:13]([NH:12][S:8]([C:4]3[CH:3]=[N:2][CH:7]=[CH:6][CH:5]=3)(=[O:10])=[O:9])[CH:18]=[CH:17][CH:16]=2)[CH3:20])[CH:27]=[N:26][CH:25]=1参加物
6
反応物 3
生成物 1
試薬・触媒・溶媒 2
実験手順
To a suspension of pyridine-3-sulfonylchloride hydrochloride (94 mg, 0.44 mmol) and N-[(1S)-1-(3-aminophenyl)ethyl]-6-chloropyrazin-2-amine (100 mg, 0.4 mmol) in dichloromethane (5 mL) was added triethylamine (0.17 mL, 1.2 mmol) dropwise at room temperature and the mixture was stirred for 17 hours. After this time the mixture was diluted with ethyl acetate (20 mL), washed successively with saturated aqueous sodium hydrogen carbonate (2×20 mL) and brine (20 mL), dried (Na2SO4) and concentrated under reduced pressure to give a yellow oil which was purified by flash chromatography (silica, ethyl acetate/hexanes) to give N-(3-{(1S)-1-[(6-chloropyrazin-2-yl)amino]ethyl}phenyl)pyridine-3-sulfonamide (44 mg, 28%) as a pale yellow foam.
後処理
- washwashed successively with saturated aqueous sodium hydrogen carbonate (2×20 mL) and brine (20 mL)
- dry with materialdried (Na2SO4)
- concentrationconcentrated under reduced pressure
- customto give a yellow oil which
- customwas purified by flash chromatography (silica, ethyl acetate/hexanes)
出典と根拠
- ORDレコード
- ord-7a9cede1e5ee4d758212fa9731856dc6
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09029386B2
関連ノート
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