Chlorotrimethylsilane → Methyl 2-Fluoro-5-nitrobenzoate
反応式
[F:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].Cl[Si](C)(C)[CH3:16].CCCCCCC>CO>[CH3:16][O:5][C:4](=[O:6])[C:3]1[CH:7]=[C:8]([N+:11]([O-:13])=[O:12])[CH:9]=[CH:10][C:2]=1[F:1]参加物
5
実験手順
To a solution of 2-fluoro-5-nitrobenzoic acid 10-1 (5.22 g, 28.2 mmol) in methanol (30 mL) was added chlorotrimethylsilane 10-2 (6.00 g, 1.96 eq.). The reaction mixture was stirred under reflux during 16 h, then cooled down to room temperature, concentrated and the resulting precipitate was filtered off, washed with a small quantity of methanol, then heptane, to provide 4.36 g (78% yield) of 2-fluoro-5-nitro-benzoic acid methyl ester 10-3 as a white powder; m/z=200 (M+H)+.
後処理
- temperatureunder reflux during 16 h
- concentrationconcentrated
- filtrationthe resulting precipitate was filtered off
- washwashed with a small quantity of methanol
出典と根拠
- ORDレコード
- ord-72d09bedf9c149588ed3642932685fcc
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08524716B2
反応ノート
読み込み中…