反应详情

温度

60 °C

A mixture of 4-iodoaniline (208 g) (available from Aldrich) and diethyl (ethoxymethylene)malonate (210 ml) (available from Aldrich) was heated to ca. 60° C., whereupon the mixture set solid. Heating was continued to 100° C., and then the mixture was removed from heating and broken up. Heating was continued at 100° C. for 1 h, and the solid was collected, washed with cyclohexane (1 L) and ethanol (2×500 ml), and dried in vacuo at 40° C. overnight to give the title compound as a white solid (356 g).

1. temperatureHeating
2. customwas continued to 100° C.
3. customthe mixture was removed
4. temperaturefrom heating
5. temperatureHeating
6. customthe solid was collected
7. washwashed with cyclohexane (1 L) and ethanol (2×500 ml)
8. customdried in vacuo at 40° C. overnight