Reaktionsgleichung
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([CH3:12])[CH:6]=[CH:5]2.[N+:13]([O-])([O-:15])=[O:14].[K+].[OH-].[Na+]>S(=O)(=O)(O)O>[N+:13]([C:3]1[C:2]([Cl:1])=[CH:11][CH:10]=[C:9]2[C:4]=1[CH:5]=[CH:6][C:7]([CH3:12])=[N:8]2)([O-:15])=[O:14]Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
6-Chloroquinaldine (11 g) was dissolved in 15 ml of concentrated sulfuric acid and the solution was ice-cooled. Then, a solution of 7.1 g of potassium nitrate dissolved in 20 ml of concentrated sulfuric acid was added to the solution dropwise, during which operation the reaction temperature was maintained at 10° C. or less. After completion of addition the mixture was agitated at the same temperature as above for 1 hour and then poured onto 200 g of ice. Subsequently, the mixture was rendered alkaline with 10% sodium hydroxide, taking care that the internal temperature should not be raised to above 20° C., thus forming a pale yellow precipitate. The precipitate was collected by filtration, washed with water and recrystallized from ethanol to obtain 12.3 g of 5-nitro-6-chloroquinaldine as pale yellow rhombic crystals having a melting point of 123° to 124° C.
Aufarbeitung
- temperaturecooled
- additionwas added to the solution dropwise
- temperatureduring which operation the reaction temperature was maintained at 10° C. or less
- additionAfter completion of addition the mixture
- temperaturebe raised to above 20° C.
- customthus forming a pale yellow precipitate
- filtrationThe precipitate was collected by filtration
- washwashed with water
- customrecrystallized from ethanol
Quellen und Nachweise
- ORD-Eintrag
- ord-b34afdba5e95464583f932dd7345f107
- Quelldatensatz
- uspto-grants-1983_11
- Patentnummer
- US04416884
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