Ethyl Acetate → 3-Fluoro-5-methoxy-4-nitrobenzonitrile
反応式
Br[C:2]1[CH:3]=[C:4]([O:12][CH3:13])[C:5]([N+:9]([O-:11])=[O:10])=[C:6]([F:8])[CH:7]=1.[C:14]([Cu])#[N:15].C(OCC)(=O)C>CN(C=O)C>[F:8][C:6]1[CH:7]=[C:2]([CH:3]=[C:4]([O:12][CH3:13])[C:5]=1[N+:9]([O-:11])=[O:10])[C:14]#[N:15]参加物
5
反応条件
- 温度
- 160 °C
実験手順
A mixture of 5-bromo-1-fluoro-3-methoxy-2-nitrobenzene (1.5 g, 6 mmol), and CuCN (698 mg, 7.8 mmol) in 10 mL of DMF was heated in a sealed tube at 160° C. overnight. It was then cooled down, diluted to ethyl acetate, washed by brine and water. The organic extract was dried and concentrated to a red solid (1 g, 85%) which was used for next step without further purification. 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 4.01 (s, 3H) 7.14 (s, 1H) 7.17 (d, J=8 Hz, 1H).
後処理
- temperatureIt was then cooled down
- washwashed by brine and water
- extractionThe organic extract
- customwas dried
- concentrationconcentrated to a red solid (1 g, 85%) which
- customwas used for next step without further purification
出典と根拠
- ORDレコード
- ord-e6ba10659c794ca29906494181c1abd9
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08026234B2
反応ノート
読み込み中…