反应详情

To a solution of sodium ethoxide at 18° prepared from sodium (41 g., 1.78 g-atoms) in ethanol (1 l.), was added a solution of 2-ethoxybenzamidine fluorosulfonate (206.5 g., 0.78 mole) in ethanol (500 ml.). The resulting solution was cooled to 13° and then treated with a solution of diethyl ethoxymethylenemalonate (180 ml., 0.89 mole) in ethanol (400 ml.). The mixture was heated under reflux for 2.25 hours. The mixture was cooled to 10° and then poured into cold water (5 l.) with good stirring. Ice was added as necessary to keep the temperature of the mixture below 20°. the mixture was acidified to pH 5 with glacial acetic acid. The solid material was collected by filtration, washed with water, and dried to give the title compound (218.7 g., 97%). Recrystallization from acetonitrile gave product with m.p. 144°-147°.

1. temperatureThe resulting solution was cooled to 13°
2. temperatureThe mixture was heated
3. temperatureunder reflux for 2.25 hours
4. temperatureThe mixture was cooled to 10°
5. additionIce was added as necessary
6. customthe temperature of the mixture below 20°
7. filtrationThe solid material was collected by filtration
8. washwashed with water
9. customdried