反応式
[C:1](Cl)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N:10]1([CH2:16][C:17]2[CH:22]=[CH:21][N:20]=[C:19]([O:23][CH2:24]/[CH:25]=[CH:26]\[CH2:27][NH:28][C:29](=[O:35])[CH2:30][S:31][CH2:32][CH2:33][OH:34])[CH:18]=2)[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1>N1C=CC=CC=1>[N:10]1([CH2:16][C:17]2[CH:22]=[CH:21][N:20]=[C:19]([O:23][CH2:24]/[CH:25]=[CH:26]\[CH2:27][NH:28][C:29](=[O:35])[CH2:30][S:31][CH2:32][CH2:33][O:34][C:1](=[O:8])[C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[CH:18]=2)[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1参加物
実験手順
0.24 ml of benzoyl chloride was added, whilst ice-cooling, to a mixture of 0.40 g of N-[4-(4-piperidinomethyl -2-pyridyloxy)-cis-2-butenyl]-2-(2-hydroxyethylthio)acetamide (prepared as described in Example 1) and 1.02 ml of pyridine, and the resulting mixture was stirred at room temperature for 2 hours. At the end of this time, the mixture was concentrated by evaporation under reduced pressure. The concentrate was diluted with water and made alkaline by the addition of an aqueous ammonia solution, after which it 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 1:40 by volume mixture of methanol and ethyl acetate as the eluent, to give 0.31 g of the title compound in a 61% yield.
後処理
- concentrationAt the end of this time, the mixture was concentrated by evaporation under reduced pressure
- additionThe concentrate was diluted with water
- additionby the addition of an aqueous ammonia solution
- extractionafter which it 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 ethyl acetate as the eluent
出典と根拠
- ORDレコード
- ord-3359d1534e2248b0acdef42c9bd27b85
- 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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