4-Phenoxyphenol → 2-Fluoro-4-phenoxyphenol
反応式
[O:1]([C:8]1[CH:13]=[CH:12][C:11]([OH:14])=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[O-]S(C(F)(F)[F:20])(=O)=O.ClC1C=[N+](F)C=C(Cl)C=1>ClCCl>[F:20][C:10]1[CH:9]=[C:8]([O:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH:13]=[CH:12][C:11]=1[OH:14]参加物
4
実験手順
To a 250 ml dichloromethane solution of 4-phenoxyphenol (2 g, 10.7 mmol) was added 3,5-dichloro-1-fluoro-pyridinium triflate (4.14 g, 13.1 mmol). After heating to reflux for 1 hr, the solvent was removed, the crude product was diluted with AcOEt and sat. bicarb. solution. The organic layer was separated, dried over anhydrous Na2SO4, filtered, concentrated, and chromatographed on silica gel. Elution with 10% methy t-butyl ether/hexanes gave 312 mg of the title compound as a pale yellow oil.
後処理
- temperatureAfter heating
- temperatureto reflux for 1 hr
- customthe solvent was removed
- additionthe crude product was diluted with AcOEt and sat. bicarb
- customThe organic layer was separated
- dry with materialdried over anhydrous Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customchromatographed on silica gel
- washElution with 10% methy t-butyl ether/hexanes
出典と根拠
- ORDレコード
- ord-08107118c1c747118a46f81b0a91fd72
- 出典データセット
- uspto-grants-2003_11
- 特許番号
- US06645997B2
反応ノート
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