Tetrafluoroboric acid → 3-Bromo-6-fluoro-2,4-dimethylpyridine
反応式
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]参加物
5
反応条件
- 温度
- 0 °C
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-e59142eaa1af4fccb70993bcebb01828
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08563565B2
反応ノート
読み込み中…