Reaktionsgleichung
[CH2:1]([O:3][CH:4]([O:9][CH2:10][CH3:11])[CH2:5][CH2:6][CH2:7][NH2:8])[CH3:2].[S:12](Cl)([OH:15])(=O)=[O:13].[CH:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>>[CH2:10]([O:9][CH:4]([O:3][CH2:1][CH3:2])[CH2:5][CH2:6][CH2:7][NH:8][S:12]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)(=[O:15])=[O:13])[CH3:11]Komponenten
3
Versuchsvorschrift
42 g 4-amino butyraldehyde diethyl acetal and 88 g benzene sulfochloride are processed as explained in Preparation Example 1. The reaction mixture is not clear from the very beginning and vigorous stirring is therefore indispensable. Methylene chloride is used for the extraction of the sulfonamide acetal. Yield: 86% based on the amino acetal used. The product will crystallize when standing for an extended time at room temperature; melting point: 109°-111°° C.; for further purification recrystallization from a 2:1 volume mixture of water and ethanol is possible.
Aufarbeitung
- customas explained in Preparation Example 1
- extractionMethylene chloride is used for the extraction of the sulfonamide acetal
- customThe product will crystallize when
- customstanding for an extended time at room temperature
- customfor further purification recrystallization
- additionfrom a 2:1 volume mixture of water and ethanol
Quellen und Nachweise
- ORD-Eintrag
- ord-f479b9f1c492412d8f65bb6cdc580c4f
- Quelldatensatz
- uspto-grants-1997_12
- Patentnummer
- US05698360
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