Reaktionsgleichung
[C:1](Cl)(=[O:3])[CH3:2].[Cl-].[Al+3].[Cl-].[Cl-].[N+](C1C=CC=CC=1)([O-])=O.[CH2:18]([N:20]1[C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH2:22][C:21]1=[O:29])[CH3:19]>>[CH2:18]([N:20]1[C:28]2[C:23](=[CH:24][C:25]([C:1](=[O:3])[CH3:2])=[CH:26][CH:27]=2)[CH2:22][C:21]1=[O:29])[CH3:19]Komponenten
5
Reaktionsbedingungen
- Temperatur
- 45 °C
Versuchsvorschrift
To a mixture of 29.25 g. (0.373 mole) of acetyl chloride and 65.9 g. of aluminum chloride in 60 ml. of nitrobenzene was added gradually 20.0 (0.124 mole) of 1-ethyloxindole. The reaction warmed to about 45° C. with an evolution of gas. After stirring for one hour the reaction was heated to 100° C. for one hour and allowed to stir at room temperature over night. The reaction mixture was poured into 2 l. of ice with stirring. After 30 minutes the product was filtered, air dried and dissolved in 200 ml. of methylene chloride. The solution was dried over magnesium sulfate and concentrated to dryness. The residue was recrystallized from toluene, 14.44 g. (57.3% yield), m.p. 141°-145° C.
Aufarbeitung
- additionTo a mixture of 29.25 g
- temperaturewas heated to 100° C. for one hour
- stirringto stir at room temperature over night
- additionThe reaction mixture was poured into 2 l
- stirringof ice with stirring
- filtrationAfter 30 minutes the product was filtered
- customair dried
- dissolutiondissolved in 200 ml
- dry with materialThe solution was dried over magnesium sulfate
- concentrationconcentrated to dryness
- customThe residue was recrystallized from toluene, 14.44 g
Quellen und Nachweise
- ORD-Eintrag
- ord-cd5efd8eaf214fefa25af3f3f35f904d
- Quelldatensatz
- uspto-grants-1987_02
- Patentnummer
- US04644005
Verknüpfte Notizen
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