Reaktionsgleichung
[C:1](Cl)(=[O:4])[CH2:2][CH3:3].[N:6]1([CH2:12][C:13]2[CH:18]=[CH:17][N:16]=[C:15]([O:19][CH2:20]/[CH:21]=[CH:22]\[CH2:23][NH:24][C:25](=[O:31])[CH2:26][S:27][CH2:28][CH2:29][OH:30])[CH:14]=2)[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1.C(=O)([O-])O.[Na+]>N1C=CC=CC=1>[N:6]1([CH2:12][C:13]2[CH:18]=[CH:17][N:16]=[C:15]([O:19][CH2:20]/[CH:21]=[CH:22]\[CH2:23][NH:24][C:25](=[O:31])[CH2:26][S:27][CH2:28][CH2:29][O:30][C:1](=[O:4])[CH2:2][CH3:3])[CH:14]=2)[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1Komponenten
Versuchsvorschrift
0.09 ml of propionyl chloride was added 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 allowed to stand at room temperature for 2 hours. At the end of this time, the reaction mixture was poured into ice-water, and a saturated aqueous solution of sodium hydrogencarbonate was added to the resulting mixture, after which it was extracted with chloroform. The extract was concentrated by evaporation under reduced pressure and the residue was purified by column chromatography through silica gel, using a 1:19 by volume mixture of methanol and ethyl acetate as the eluent, to give 0.39 g (yield 85%) of the title compound as an oil.
Aufarbeitung
- extractionafter which it was extracted with chloroform
- concentrationThe extract was concentrated by evaporation under reduced pressure
- customthe residue was purified by column chromatography through silica gel
- additionby volume mixture of methanol and ethyl acetate as the eluent
Quellen und Nachweise
- ORD-Eintrag
- ord-0d44a03b9b0e4691a156f7a6265534b7
- Quelldatensatz
- uspto-grants-1997_04
- Patentnummer
- US05616579
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