反応式
[CH2:1]([O:3][C:4]([N:6]1[CH2:11][CH2:10][CH:9]([NH:12][CH2:13][C:14]2[CH:19]=[CH:18][N:17]=[C:16]([C:20]3[CH:25]=[C:24]([O:26][CH3:27])[C:23]([O:28][CH3:29])=[C:22]([O:30][CH3:31])[CH:21]=3)[CH:15]=2)[CH2:8][CH2:7]1)=[O:5])[CH3:2].C(=O)([O-])[O-].[K+].[K+].I[CH2:39][CH3:40]>C(#N)C>[CH2:1]([O:3][C:4]([N:6]1[CH2:11][CH2:10][CH:9]([N:12]([CH2:39][CH3:40])[CH2:13][C:14]2[CH:19]=[CH:18][N:17]=[C:16]([C:20]3[CH:21]=[C:22]([O:30][CH3:31])[C:23]([O:28][CH3:29])=[C:24]([O:26][CH3:27])[CH:25]=3)[CH:15]=2)[CH2:8][CH2:7]1)=[O:5])[CH3:2]参加物
5
反応条件
- 温度
- 80 °C
実験手順
To a solution of 1-(ethoxycarbonyl)-4-[[2-(3,4,5-trimethoxyphenyl)pyridin-4-yl]methylamino]piperidine (400 mg) in acetonitrile (5 mL) was added potassium carbonate (13 mg) and iodoethane (145 mg). The mixture was placed in sealed vessel and stirred at 80° C. for 2 hours. After removing the solvent in vacuo, ethyl acetate was added, washed with water and brine, dried over anhydrous sodium sulfate and evaporated. The residue was subjected to a column of silica gel using chloroform-methanol (30:1) as an eluent. Fractions containing the product were collected and evaporated to give the title compound as yellow syrup.
後処理
- customThe mixture was placed in sealed vessel
- customAfter removing the solvent in vacuo, ethyl acetate
- additionwas added
- washwashed with water and brine
- dry with materialdried over anhydrous sodium sulfate
- customevaporated
- additionFractions containing the product
- customwere collected
- customevaporated
出典と根拠
- ORDレコード
- ord-d97de50a70584570bf35d644cffd7a87
- 出典データセット
- uspto-grants-2002_12
- 特許番号
- US06498169B1
関連ノート
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