反応式
[N:1]1([CH2:7][C:8]2[CH:13]=[CH:12][N:11]=[C:10]([O:14][CH2:15][CH2:16][CH2:17][NH2:18])[CH:9]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[O:19]1[CH2:24][CH2:23][S:22][CH2:21][C:20]1=[O:25]>C(O)C>[N:1]1([CH2:7][C:8]2[CH:13]=[CH:12][N:11]=[C:10]([O:14][CH2:15][CH2:16][CH2:17][NH:18][C:20](=[O:25])[CH2:21][S:22][CH2:23][CH2:24][OH:19])[CH:9]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1参加物
4
実験手順
A mixture of 0.38 g of 3-(4-piperidinomethyl-2-pyridyloxy)propylamine and 0.18 g of 1,4-oxathian-2-one was added to 10 ml of ethanol, and the resulting mixture was heated under reflux for 2 hours. At the end of this time, the reaction mixture was concentrated by evaporation under reduced pressure. The concentrate was mixed with water, and the resulting aqueous mixture was extracted with ethyl acetate. The extract was concentrated by evaporation under reduced pressure, and the concentrate was purified by column chromatography through silica gel, using a 1:9 by volume mixture of methanol and methylene chloride as the eluent, to give 0.49 g (yield 88%) of the title compound as an oil.
後処理
- temperaturethe resulting mixture was heated
- temperatureunder reflux for 2 hours
- concentrationAt the end of this time, the reaction mixture was concentrated by evaporation under reduced pressure
- additionThe concentrate was mixed with water
- extractionthe resulting aqueous mixture was extracted with ethyl acetate
- concentrationThe extract was concentrated by evaporation under reduced pressure
- customthe concentrate was purified by column chromatography through silica gel
- additionby volume mixture of methanol and methylene chloride as the eluent
出典と根拠
- ORDレコード
- ord-6d43970eb09d4df986664b94bf5d6cb2
- 出典データセット
- uspto-grants-1997_04
- 特許番号
- US05616579
関連ノート
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