Reaktionsgleichung
Cl.[N:2]1([CH2:8][CH2:9][C:10]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=O)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.Cl.[NH2:19][OH:20].C(=O)([O-])O.[Na+].[OH-].[Na+]>O.[Ag]>[N:2]1([CH2:8][CH2:9][C:10](=[N:19][OH:20])[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
In 470 ml of water were dissolved 60.2 g of β-piperidinopropiophenone hydrochloride and 18.1 g of hydroxylamine hydrochloride. To this solution was added portionwise 21.9 g of sodium hydrogencarbonate. After the whole amount was added, the mixture was stirred overnight. To the stirred mixture was then added an aqueous solution of 14.2 g of sodium hydroxide in 47 ml of water. Thus obtained mixture was well stirred and allowed to stand for 2 hours to produce a white precipitate. The precipitate was collected by filtration and washed successively with two portions of 200 ml of water and ethanol. The washed precipitate was dried to obtain a white solid. The solid was then recrystallized from methanol to obtain 41.2 g (yield: 74.8%) of the subject compound as a silver-white scaly product.
Aufarbeitung
- additionAfter the whole amount was added
- stirringThus obtained mixture was well stirred
- waitto stand for 2 hours
- customto produce a white precipitate
- filtrationThe precipitate was collected by filtration
- washwashed successively with two portions of 200 ml of water and ethanol
- customThe washed precipitate was dried
- customto obtain a white solid
- customThe solid was then recrystallized from methanol
Quellen und Nachweise
- ORD-Eintrag
- ord-e9c738adc29e404d9db764e041f0902d
- Quelldatensatz
- uspto-grants-1988_08
- Patentnummer
- US04764617
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