反应详情

To a stirred mixture of 4-bromophenyl-acetamidine (11.25 g, 0.04 mole) and 1-dimethylamino-3-dimethylimonio-1-(4-bromophenyl)-1-propane perchlorate (15.25 g, 0.04 mole) in 100 mL of dry ethanol is added 0.04 mole sodium ethoxide (prepared from 0.92 g Na and 65 mL ethanol). After stirring for 30 min at room temperature a further equivalent of sodium ethoxide is added, and the mixture is heated under reflux for 2 hr. The solvent is removed under reduced pressure, and the yellow-brown residue triturated with 150 mL water. The solid is filtered, washed with water, dried in air and recrystallized from ether:hexane (1:3) to give 12.5 g (77%) of a pale yellow crystalline solid, mp 93°-94° C.

1. additionis added
2. temperaturethe mixture is heated
3. temperatureunder reflux for 2 hr
4. customThe solvent is removed under reduced pressure
5. customthe yellow-brown residue triturated with 150 mL water
6. filtrationThe solid is filtered
7. washwashed with water
8. customdried in air
9. customrecrystallized from ether:hexane (1:3)