反応式
[C:1]1(/[C:7](/[CH3:14])=[CH:8]/[C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.N(C(C)(C)C#N)=NC(C)(C)C#N.[Br:27]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl>[Br:27][CH2:14]/[C:7](/[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)=[CH:8]/[C:9]([O:11][CH2:12][CH3:13])=[O:10]参加物
5
反応条件
- 温度
- 75 °C
実験手順
A mixture of 14 g (74 mmol) of ethyl (E)-3-phenylbut-2-enoate, 0.47 g of 2,2′-azobis(2-methylpropionitrile) and 330 ml of carbon tetrachloride is heated to 75° C. 19.8 g (111 mmol) of N-bromosuccinimide are added portionwise at this temperature. The mixture is then refluxed for five hours. The insoluble material is filtered off at 25° C. The filtrate is washed with water and dried over Na2SO4; the solvents are evaporated off (orange-coloured oil: 19.7 g; 99%).
後処理
- temperatureThe mixture is then refluxed for five hours
- filtrationThe insoluble material is filtered off at 25° C
- washThe filtrate is washed with water
- dry with materialdried over Na2SO4
- customthe solvents are evaporated off (orange-coloured oil: 19.7 g; 99%)
出典と根拠
- ORDレコード
- ord-33c95e91bcc34572aa32018660fd2a43
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07737176B2
関連ノート
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