反应详情

温度

95 °C

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%.

1. customequipped with a condenser, addition funnel, and magnetic bar
2. stirringthe flask stirred at 50° C
3. temperaturethe mixture was refluxed for 6 hrs
4. temperatureto cool to room temperature
5. temperatureThe mixture was again refluxed for 8 hrs
6. temperatureThe solution was cooled to room temperature
7. customTHF was evaporated
8. washThe solid was washed thoroughly with dilute HCl and water
9. customThe product was recrystallized in 95% methanol