Potassium Carbonate → 2-(4-Chloro-2,6-dimethylphenoxy)acetonitrile
反応式
[Cl:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([OH:9])=[C:4]([CH3:10])[CH:3]=1.Br[CH2:12][C:13]#[N:14].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Cl:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([O:9][CH2:12][C:13]#[N:14])=[C:4]([CH3:10])[CH:3]=1参加物
5
実験手順
4-Chloro-2,6-dimethylphenol (5.0 g, 32 mmol), bromoacetonitrile (2.2 mL, 32 mmol) and potassium carbonate (6.6 g, 48 mmol) are combined with acetone (50 mL) and heated at reflux for 18 h. The reaction is filtered, concentrated and the residue partitioned between dichloromethane and water. The organic phase is washed with 1N HCl and water and is then dried over magnesium sulfate, concentrated and purified by column chromatography (silica, 10% ethyl acetate in hexanes) to provide the title compound. MS (EI) 195 (M)+, Cl pattern.
後処理
- temperatureheated
- temperatureat reflux for 18 h
- filtrationThe reaction is filtered
- concentrationconcentrated
- customthe residue partitioned between dichloromethane and water
- washThe organic phase is washed with 1N HCl and water
- dry with materialis then dried over magnesium sulfate
- concentrationconcentrated
- custompurified by column chromatography (silica, 10% ethyl acetate in hexanes)
出典と根拠
- ORDレコード
- ord-af85560a598a444884c6534111ba0589
- 出典データセット
- uspto-grants-2003_10
- 特許番号
- US06635655B1
反応ノート
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