Chloromethyl Methyl Ether → 4-Fluoro-2-methoxymethoxy-1-nitro-benzene
反応式
[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]=1参加物
6
実験手順
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.
後処理
- washwashed with brine
- concentrationconcentrated in vacuo
- customto give a crude residue, which
- customwas purified by column chromatography (silica 5-25% EtOAc/hexane)
出典と根拠
- ORDレコード
- ord-642935e779634632ab0d956e307a76ad
- 出典データセット
- uspto-grants-2007_11
- 特許番号
- US07294635B2
反応ノート
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