1-Bromo-4-fluoro-2-methyl-5-nitrobenzene → 5-Bromo-2-fluoro-4-methylaniline
反応式
[Br:1][C:2]1[CH:7]=[C:6]([N+:8]([O-])=O)[C:5]([F:11])=[CH:4][C:3]=1[CH3:12].[H][H]>[Ni].C(O)C>[Br:1][C:2]1[C:3]([CH3:12])=[CH:4][C:5]([F:11])=[C:6]([CH:7]=1)[NH2:8]参加物
5
実験手順
Combine crude 1-bromo-4-fluoro-2-methyl-5-nitrobenzene (32.4 g, 138 mmol), ethanol (100 mL) and Raney Nickel (1.00 g, 17.04 mmol) in a shaker flask. Charge the flask with hydrogen (275 kPa) and agitate until the absorption of hydrogen ceases. De-pressurize the reaction vessel, remove the catalyst by filtration, and evaporate the filtrate to dryness. Add MTBE, then filter again and evaporate the filtrate. Stir residue in hexanes. Collect the solids by filtration, wash with cold hexanes and dry in vacuo to provide the title compound (17.8 g, 63% yield) as a dark solid. MS (m/z): 204.0 (M+1)/206.0 (M+3).
後処理
- customDe-pressurize the reaction vessel, remove the catalyst
- filtrationby filtration
- customevaporate the filtrate to dryness
- filtrationAdd MTBE, then filter again
- customevaporate the filtrate
- customCollect the solids
- filtrationby filtration
- washwash with cold hexanes
- customdry in vacuo
出典と根拠
- ORDレコード
- ord-ee685ee613564d3fa6d76b9da194d191
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09334267B2
反応ノート
読み込み中…