Pyrazole → 5-Bromo-2-(1H-pyrazol-1-yl)pyridine
反応式
[NH:1]1[CH:5]=[CH:4][CH:3]=[N:2]1.[H-].[Na+].Br[C:9]1[CH:14]=[CH:13][C:12]([Br:15])=[CH:11][N:10]=1>CN(C=O)C>[Br:15][C:12]1[CH:13]=[CH:14][C:9]([N:1]2[CH:5]=[CH:4][CH:3]=[N:2]2)=[N:10][CH:11]=1参加物
5
実験手順
Pyrazole (2.05 g, 30.11 mol) was added in portions to sodium hydride (60% in oil, 1.20 g, 30.00 mmol) in DMF (40 mL) and the resulting mixture was stirred for 1 h at RT. 2,5-Dibromopyridine (4.75 g, 20.05 mmol) was added and the mixture was heated to 100° C. for 2 h. Ice-water (100 mL) was added to the cooled reaction mixture and the precipitated solids were removed by filtration and allowed to air-dry. Recrystallization from hexane provided 3.31 g (74%) of the title compound as a tan solid. MS 224 (M+H)+.
後処理
- temperaturethe mixture was heated to 100° C. for 2 h
- customthe precipitated solids were removed by filtration
- customto air-dry
- customRecrystallization from hexane
出典と根拠
- ORDレコード
- ord-d42a361bbd204cae93b28e0687e6bc81
- 出典データセット
- uspto-grants-2003_09
- 特許番号
- US06613747B2
反応ノート
読み込み中…