Ammonium Hydroxide → 3-Bromo-2,5,6-trifluoroaniline
反応式
[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[C:4](F)[C:3]=1[F:11].[OH-].[NH4+:13]>O>[Br:1][C:2]1[C:3]([F:11])=[C:4]([C:5]([F:9])=[C:6]([F:8])[CH:7]=1)[NH2:13]参加物
4
反応条件
- 温度
- 150 °C
実験手順
To a microwave tube was added 1-bromo-2,3,4,5-tetrafluorobenzene (1.0 g) and 28% aqueous ammonium hydroxide (5 mL). The mixture was heated under microwave irradiation at 150° C. for 2 hrs, then the mixture was poured into water and extracted with hexane. The organic layer was separated, dried with MgSO4, then concentrated. The residue was purified by silica gel flash chromatography (9:1 hexanes/ethyl acetate eluant) afford the title compound as a colorless liquid. 1H NMR (400 MHz, CDCl3) δ 6.75 (m, 1H), 3.95 (br s, 2H) ppm; MS m/z: 226, 228 (M+H)+.
後処理
- extractionextracted with hexane
- customThe organic layer was separated
- dry with materialdried with MgSO4
- concentrationconcentrated
- customThe residue was purified by silica gel flash chromatography (9:1 hexanes/ethyl acetate eluant)
出典と根拠
- ORDレコード
- ord-23f3f13629044334ab0d0d2f4e93f6cd
- 出典データセット
- uspto-grants-2016_04
- 特許番号
- US09314464B2
反応ノート
読み込み中…