Cornforth reagent → 1-(4-Bromo-3-fluorophenyl)ethan-1-one
反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([OH:10])[CH3:9])=[CH:4][C:3]=1[F:11].[Cr](O[Cr]([O-])(=O)=O)([O-])(=O)=O.[NH+]1C=CC=CC=1.[NH+]1C=CC=CC=1>C(Cl)Cl>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:10])[CH3:9])=[CH:4][C:3]=1[F:11]参加物
4
実験手順
To a solution of crude 1-(4-bromo-3-fluorophenyl)ethanol oil (from Step 1) in DCM (100 mL) was added pyridinium dichromate (8.96 g, 23.82 mmol). The mixture was stirred overnight at room temperature. To the mixture was added celite, the reaction mixture was filtered through a celite pad and rinsed several times with DCM. The filtrate was concentrated under reduced pressure. The crude material was purified by column chromatography [SiO2, 40 g, heptane/ethyl acetate] providing 1-(4-bromo-3-fluorophenyl)ethanone (3.08 g) as a white solid.
後処理
- additionTo the mixture was added celite
- filtrationthe reaction mixture was filtered through a celite pad
- washrinsed several times with DCM
- concentrationThe filtrate was concentrated under reduced pressure
- customThe crude material was purified by column chromatography [SiO2, 40 g, heptane/ethyl acetate]
出典と根拠
- ORDレコード
- ord-f098ac911451486585d6a41adb82968f
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09434719B2
反応ノート
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