Reaktionsgleichung
[N+:1]([C:4]1[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=1[NH2:6])([O-:3])=[O:2].[CH3:11][C:12]([CH2:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[CH2:13]>[Cl-].[Zn+2].[Cl-]>[C:12]([C:9]1[CH:8]=[CH:7][C:5]([NH2:6])=[C:4]([N+:1]([O-:3])=[O:2])[CH:10]=1)([CH2:14][C:15]([CH3:18])([CH3:17])[CH3:16])([CH3:13])[CH3:11]Komponenten
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 60 °C
Versuchsvorschrift
In a 2-liter reaction flask fitted with a condenser, nitrogen inlet, stirrer, thermometer and addition funnel is placed 272 grams (2.0 moles) of anhydrous zinc chloride. The flask is placed under a nitrogen atmosphere and 166 ml (2.0 moles) of concentrated (12 N) hydrochloric acid is added over a 10-minute period with the temperature rising from 22° to 40° C. To this is then added 276 grams (2.0 moles) of o-nitroaniline over a 15-minute period to avoid the formation of lumps. The resulting thick red slurry is heated to 60° C. and then 474 grams (3.0 moles) of diisobutylene is added gradually over a 110-minute period with the temperature rising during this period from 60° to 90° C. The deep red fluid reaction mixture is heated for another 18 hours at reflux till only a trace of o-nitroaniline is observed by thin layer chromatography.
Aufarbeitung
- customIn a 2-liter reaction flask
- customfitted with a condenser, nitrogen inlet, stirrer
- additionthermometer and addition funnel
- concentration166 ml (2.0 moles) of concentrated (12 N) hydrochloric acid
- additionis added over a 10-minute period with the temperature
- customrising from 22° to 40° C
- waitrising during this period from 60° to 90° C
- customThe deep red fluid reaction mixture
- temperatureis heated for another 18 hours
Quellen und Nachweise
- ORD-Eintrag
- ord-3497fce3c27c4a8183dd59dfdd64c3b5
- Quelldatensatz
- uspto-grants-1988_02
- Patentnummer
- US04727158
Verknüpfte Notizen
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