Tetrafluoroboric acid → 3-Bromo-6-fluoro-2,4-dimethylpyridine
반응식
N[C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([Br:9])=[C:4]([CH3:10])[N:3]=1.N([O-])=O.[Na+].[F:15][B-](F)(F)F.[H+]>O>[Br:9][C:5]1[C:4]([CH3:10])=[N:3][C:2]([F:15])=[CH:7][C:6]=1[CH3:8]참가 물질
5
반응 조건
- 온도
- 0 °C
실험 절차
2-amino-5-bromo-4,6-dimethylpyridine (2 g) was suspended in fluoroboric acid (48% aqueous solution, 7.5 mL). Sodium nitrite (890 mg) dissolved in water (3 mL) was added to the solution at 0° C. The reaction mixture was stirred at 0° C. for 10 minutes. The precipitated solid was collected by filtration and suspended in n-heptane (100 mL). The solution was stirred with heating under reflux for two hours. After cooling to room temperature, the precipitated solid was collected by filtration. The resulting solid was dried under reduced pressure to give the title compound (500 mg).
후처리
- additionwas added to the solution at 0° C
- filtrationThe precipitated solid was collected by filtration
- stirringThe solution was stirred
- temperaturewith heating
- temperatureunder reflux for two hours
- temperatureAfter cooling to room temperature
- filtrationthe precipitated solid was collected by filtration
- customThe resulting solid was dried under reduced pressure
출처 및 근거
- ORD 기록
- ord-e59142eaa1af4fccb70993bcebb01828
- 출처 데이터셋
- uspto-grants-2013_10
- 특허 번호
- US08563565B2
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