Reaktionsgleichung
[H-].[Na+].[N+:3]([C:6]1[CH:11]=[CH:10][C:9]([N:12]=[N:13][C:14]2[CH:20]=[CH:19][C:17]([NH2:18])=[CH:16][CH:15]=2)=[CH:8][CH:7]=1)([O-:5])=[O:4].[C:21](O)(=[O:25])[C:22]([CH3:24])=[CH2:23]>C1COCC1>[CH3:24][C:22]([C:21]([NH:18][C:17]1[CH:19]=[CH:20][C:14]([N:13]=[N:12][C:9]2[CH:10]=[CH:11][C:6]([N+:3]([O-:5])=[O:4])=[CH:7][CH:8]=2)=[CH:15][CH:16]=1)=[O:25])=[CH2:23]Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 95 °C
Versuchsvorschrift
0.6 g of sodium hydride was added carefully to a 3 neck flask equipped with a condenser, addition funnel, and magnetic bar. 75 ml of anhydrous THF was added and the mixture stirred for 10 minutes. A solution of 4.0 g 4-(4-nitrophenylazo)aniline in 75 ml THF was added drop-wise and the flask stirred at 50° C. The temperature was raised to 95° C., and the mixture was refluxed for 6 hrs. The mixture was allowed to cool to room temperature and then 6.0 g of methacrylic acid in 20 ml THF was added drop-wise. The mixture was again refluxed for 8 hrs. The solution was cooled to room temperature. THF was evaporated to reveal a dark orange solid. The solid was washed thoroughly with dilute HCl and water. The product was recrystallized in 95% methanol. The yield was 56%.
Aufarbeitung
- customequipped with a condenser, addition funnel, and magnetic bar
- stirringthe flask stirred at 50° C
- temperaturethe mixture was refluxed for 6 hrs
- temperatureto cool to room temperature
- temperatureThe mixture was again refluxed for 8 hrs
- temperatureThe solution was cooled to room temperature
- customTHF was evaporated
- washThe solid was washed thoroughly with dilute HCl and water
- customThe product was recrystallized in 95% methanol
Quellen und Nachweise
- ORD-Eintrag
- ord-9511b8526ed0454c9bd035cd15df1a1d
- Quelldatensatz
- uspto-grants-2010_11
- Patentnummer
- US07842367B2
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