Benzophenone → 3,3-Diphenylacrylonitrile
反応式
[C:1]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[K+].[C:17](#[N:19])[CH3:18]>>[C:2]1([C:1]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[CH:18][C:17]#[N:19])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1参加物
4
実験手順
To a solution of benzophenone (9.1 g, 50 mmol) in acetonitrile (20 mL) was added potassium hydroxide (3.3 g, 50 mmol) in acetonitrile (25 mL). The solution was refluxed for 8 hours. The hot reaction mixture was poured into 100 g crushed ice and then extracted with dichloromethane. The organic extract was washed with water, dried over sodium sulfate, and concentrated in vacuo. The crude material was purified by flash column chromatography (diethyl ether/hexanes) to give 3,3-diphenylacrylonitrile (7.7 g, 73.3%) as an oil.
後処理
- temperatureThe solution was refluxed for 8 hours
- additionThe hot reaction mixture was poured into 100 g
- customcrushed ice
- extractionextracted with dichloromethane
- extractionThe organic extract
- washwas washed with water
- dry with materialdried over sodium sulfate
- concentrationconcentrated in vacuo
- customThe crude material was purified by flash column chromatography (diethyl ether/hexanes)
出典と根拠
- ORDレコード
- ord-f8097f9a50d0425c96c8f703a9bad69c
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08629149B2
反応ノート
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