反応式
[CH2:1]([O:3][C:4](=[O:20])[CH2:5][C:6](=[O:19])[C:7]([C:10]1[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[C:12]([Br:18])[CH:11]=1)([CH3:9])[CH3:8])[CH3:2].C(=O)([O-])[O-].[Cs+].[Cs+].Cl[C:28]1[CH:35]=[CH:34][C:31]([C:32]#[N:33])=[CH:30][C:29]=1[N+:36]([O-:38])=[O:37].Cl>CN(C=O)C>[CH2:1]([O:3][C:4](=[O:20])[CH:5]([C:28]1[CH:35]=[CH:34][C:31]([C:32]#[N:33])=[CH:30][C:29]=1[N+:36]([O-:38])=[O:37])[C:6](=[O:19])[C:7]([C:10]1[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[C:12]([Br:18])[CH:11]=1)([CH3:9])[CH3:8])[CH3:2]参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 45 °C
実験手順
4-(3-Bromo-4-methoxy-phenyl)-4-methyl-3-oxo-pentanoic acid ethyl ester (Compound K3, 10.3 g, 30.01 mmol) was dissolved in DMF (80 mL), added with cesium carbonate (24.4 g, 2.5 eq.) and 4-chloro-3-nitro-benzonitrile (7.12 g, 1.3 eq.), and then stirred at 45° C. for 4 hr. The reaction solution was added to 1 N aqueous solution of hydrochloric acid, and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over sodium sulfate. The drying agent was removed by filtration, and after concentration under reduced pressure the title compound was obtained as a crude product (yellow oily substance).
後処理
- extractionextracted with ethyl acetate
- washThe organic layer was washed with saturated brine
- dry with materialdried over sodium sulfate
- customThe drying agent was removed by filtration
- concentrationafter concentration under reduced pressure the title compound
出典と根拠
- ORDレコード
- ord-44454808dd70496f96a693021480053d
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09440922B2
関連ノート
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