Acetyl chloride → 1-(5-Bromo-4-methylthiophen-2-yl)ethan-1-one
反応式
[C:1](Cl)(=[O:3])[CH3:2].[Al+3].[Cl-].[Cl-].[Cl-].[Br:9][C:10]1[S:11][CH:12]=[CH:13][C:14]=1[CH3:15]>ClCCl>[Br:9][C:10]1[S:11][C:12]([C:1](=[O:3])[CH3:2])=[CH:13][C:14]=1[CH3:15]参加物
5
実験手順
Acetyl chloride (7.09 g) is added to a suspension of AlCl3 (11.53 g) in dichloromethane (310 ml) at 0° C. After 45 minutes at 0° C., 2-bromo-3-methylthiophene (5.0 g) is added dropwise. After 1 hour at 0° C., the reaction is quenched by added water (100 ml). The mixture is extracted three times with dichloromethane. The organic phases are combined, dried over MgSO4 and concentrated in vacuo. The crude product is purified by chromatography on silica gel (180 g) eluting with a mixture of ethyl acetate and heptane (1:6) to yield 1-(5-bromo-4-methyl-thiophen-2-yl)-ethanone (3.5 g) as a brown solid.
後処理
- waitAfter 1 hour at 0° C.
- customthe reaction is quenched
- additionby added water (100 ml)
- extractionThe mixture is extracted three times with dichloromethane
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- customThe crude product is purified by chromatography on silica gel (180 g)
- washeluting with a mixture of ethyl acetate and heptane (1:6)
出典と根拠
- ORDレコード
- ord-867965c46b404420bd394b02d533937e
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08653116B2
反応ノート
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