Chlorotrimethylsilane → Methyl 2-Fluoro-5-nitrobenzoate
반응식
[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]참가 물질
5
실험 절차
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)+.
후처리
- temperatureunder reflux during 16 h
- concentrationconcentrated
- filtrationthe resulting precipitate was filtered off
- washwashed with a small quantity of methanol
출처 및 근거
- ORD 기록
- ord-72d09bedf9c149588ed3642932685fcc
- 출처 데이터셋
- uspto-grants-2013_09
- 특허 번호
- US08524716B2
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