Reaktionsgleichung
Cl.C(O[C:5](=[NH:16])[CH2:6][S:7]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)(=[O:9])=[O:8])C.[OH-].[Na+].C(=O)(O)[O-].[Na+].[C:24]([NH:32][NH2:33])(=[O:31])[C:25]1[CH:30]=[CH:29][CH:28]=[N:27][CH:26]=1>C(Cl)(Cl)Cl.O1CCOCC1>[NH2:16][C:5](=[N:33][NH:32][C:24](=[O:31])[C:25]1[CH:30]=[CH:29][CH:28]=[N:27][CH:26]=1)[CH2:6][S:7]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)(=[O:9])=[O:8]Komponenten
7
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
A suspension of 23.6 g (0.089 mol) 2-(phenylsulfonyl)-ethanimidic acid ethyl ester hydrochloride in 300 ml chloroform was treated with 98 ml 1N aqueous sodium hydoxide. 200 ml of a saturated aqueous sodiumbicarbonate solution was added and the mixture was extracted with chloroform. The extracts were combined and dried with sodium sulfate and the solvents were distilled off under reduced pressure. The resulting colorless oil was stirred together with 13.5 g (0.098 mol) nicotinic acid hydrazide in 500 ml dioxane over night at 50° C. The resulting precipitate was filtered off and dried. A yield of 15.5 g (55%) nicotinic acid (1-amino-2-benzenesulfonyl-ethylidene)-hydrazide was obtained as white solid, MS m/e (%): 319 (M+H+, 100).
Aufarbeitung
- extractionthe mixture was extracted with chloroform
- dry with materialdried with sodium sulfate
- distillationthe solvents were distilled off under reduced pressure
- filtrationThe resulting precipitate was filtered off
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-da3a986cd3924997b9a302428823fde1
- Quelldatensatz
- uspto-grants-2002_03
- Patentnummer
- US06355653B1
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