反応式
Cl[CH2:2][CH2:3][CH2:4][O:5][CH2:6][CH2:7][C:8]1[CH:9]=[CH:10][C:11]2[S:15][CH:14]=[CH:13][C:12]=2[CH:16]=1.[NH:17]1[CH2:20][CH:19]([NH:21][C:22](=[O:24])[CH3:23])[CH2:18]1.O.C(OCC)(=O)C>CN(C)C=O>[S:15]1[C:11]2[CH:10]=[CH:9][C:8]([CH2:7][CH2:6][O:5][CH2:4][CH2:3][CH2:2][N:17]3[CH2:20][CH:19]([NH:21][C:22](=[O:24])[CH3:23])[CH2:18]3)=[CH:16][C:12]=2[CH:13]=[CH:14]1参加物
反応条件
- 温度
- 90 °C
実験手順
In 8 mL of N,N-dimethylformamide was dissolved 0.80 g of 5-[2-(3-chloropropoxy)ethyl]-1-benzothiophene, and 1.20 g of N-(3-azetidinyl)acetamide was added to the solution, after which the resulting mixture was stirred at 90° C. for 12 hours. After the reaction mixture was cooled, water and ethyl acetate were added thereto and the organic layer was separated. The organic layer was washed with water and then a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then distilled under reduced pressure to remove the solvent. The residue was purified by a column chromatography (eluent; chloroform: methanol=7:1) to obtain 0.39 g of N-(1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-azetidinyl)acetamide as a light-yellow oil.
後処理
- additionwas added to the solution
- temperatureAfter the reaction mixture was cooled
- customthe organic layer was separated
- washThe organic layer was washed with water
- dry with materiala saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate
- distillationdistilled under reduced pressure
- customto remove the solvent
- customThe residue was purified by a column chromatography (eluent; chloroform: methanol=7:1)
出典と根拠
- ORDレコード
- ord-9164049d97e645e781188bb154a4ca36
- 出典データセット
- uspto-grants-2012_09
- 特許番号
- USRE043676E1
関連ノート
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