反応式
F[C:2]1[N:7]=[CH:6][C:5]([NH2:8])=[CH:4][CH:3]=1.[NH:9]1[CH:13]=[CH:12][CH:11]=[N:10]1.C(=O)([O-])[O-].[Cs+].[Cs+]>CN1C(=O)CCC1.C(Cl)(Cl)Cl>[N:9]1([C:2]2[N:7]=[CH:6][C:5]([NH2:8])=[CH:4][CH:3]=2)[CH:13]=[CH:12][CH:11]=[N:10]1参加物
6
反応条件
- 温度
- 120 °C
実験手順
Commercial 6-fluoropyridin-3-amine (500 mg, 4.46 mmol) was dissolved in 20 mL dry NMP. To it were added pyrazole (910 mg, 13.4 mmol) and cesium carbonate (4.4 g, 13.4 mmol). The mixture was stirred in a sealed tube at 120° C. for over the weekend (3 nights). The mixture was diluted with chloroform, washed with brine (3 times), dried, concentrated and subjected to flash column (0 to 30% EtOAc in DCM) to isolate 6-(1H-pyrazol-1-yl)pyridin-3-amine (120 mg, 17% yield).
後処理
- washwashed with brine (3 times)
- customdried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-b211c993c0db4887b1819cb46fe63efb
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846928B2
関連ノート
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