Pyrazole → 5-Bromo-2-(1H-pyrazol-1-yl)pyridine
반응식
[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]=1참가 물질
5
실험 절차
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)+.
후처리
- temperaturethe mixture was heated to 100° C. for 2 h
- customthe precipitated solids were removed by filtration
- customto air-dry
- customRecrystallization from hexane
출처 및 근거
- ORD 기록
- ord-15318dd70fb64dadb67477f070d2824e
- 출처 데이터셋
- uspto-grants-2004_11
- 특허 번호
- US06825170B2
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