Hydrogen Bromide → HCID 70097318、化合物
反応式
[CH3:1][C:2]1[CH:7]=[C:6]([NH2:8])[C:5]([CH3:9])=[CH:4][N:3]=1.OO.[BrH:12]>>[Br:12][C:7]1[C:2]([CH3:1])=[N:3][CH:4]=[C:5]([CH3:9])[C:6]=1[NH2:8]参加物
4
反応条件
- 温度
- 75 °C
実験手順
A mixture of 2,5-dimethylpyridin-4-amine (3.57 g, 29.3 mmol) in 48% hydrogen bromide aqueous solution (40 mL) was heated to 75° C. Then 15% hydrogen peroxide (7 mL) was added dropwise over 30 min. The reaction mixture was stirred at 75° C. for 1 h, and concentrated under reduced pressure. The pH of the solution was adjusted to 9 with 1 N sodium hydroxide solution. The aqueous mixture was extracted with DCM (250 mL×3), and the combined organic phase was washed with saturated sodium chloride solution (250 mL×1), dried with sodium sulfate, and concentrated to give 5.0 g of the product as a yellow solid. MS (ESI): m/z 203.1 [M+H]+.
後処理
- concentrationconcentrated under reduced pressure
- extractionThe aqueous mixture was extracted with DCM (250 mL×3)
- washthe combined organic phase was washed with saturated sodium chloride solution (250 mL×1)
- dry with materialdried with sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-580610cb250142668c939703db9787be
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08969349B2
反応ノート
読み込み中…