Chloromethyl Methyl Ether → 4-Fluoro-2-methoxymethoxy-1-nitro-benzene
반응식
[F:1][C:2]1[CH:3]=[CH:4][C:5]([N+:9]([O-:11])=[O:10])=[C:6]([OH:8])[CH:7]=1.[H-].[Na+].Cl[CH2:15][O:16][CH3:17]>C1COCC1.C(OCC)(=O)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]([N+:9]([O-:11])=[O:10])=[C:6]([O:8][CH2:15][O:16][CH3:17])[CH:7]=1참가 물질
6
실험 절차
To a solution of 5-fluoro-2-nitro-phenol (234 mg, 1.49 mmol) in 5 mL THF, sodium hydride (122 mg, 2.9 mmol) was added, followed by chloromethoxy methane (113 ul, 1.49 mmol) at 0° C. The mixture was warmed to room temperature and stirred for 10 hours, then diluted with ethyl acetate and washed with brine. The organic layers were combined and concentrated in vacuo to give a crude residue, which was purified by column chromatography (silica 5-25% EtOAc/hexane) to give 4-fluoro-2-methoxymethoxy-1-nitro-benzene.
후처리
- washwashed with brine
- concentrationconcentrated in vacuo
- customto give a crude residue, which
- customwas purified by column chromatography (silica 5-25% EtOAc/hexane)
출처 및 근거
- ORD 기록
- ord-642935e779634632ab0d956e307a76ad
- 출처 데이터셋
- uspto-grants-2007_11
- 특허 번호
- US07294635B2
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