반응식
[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]1참가 물질
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-3359d1534e2248b0acdef42c9bd27b85
- 출처 데이터셋
- uspto-grants-1997_04
- 특허 번호
- US05616579
연결된 노트
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