反应详情

Phosphorous pentachloride (9.63 g, 46.2 mmol) is added to a mixture of diethyl (4-cyano-2-fluorophenyl)methylenedicarbamate (intermediate 26, 6.50 g, 21.0 mmol) in toluene (25.0 mL), and the mixture is heated at reflux for 3 h. The toluene is evaporated, and the mixture is then purified by distillation under reduced pressure. The first fraction (ca. 35° C., ca. 0.2 mbar) is discarded. The second fraction (ca. 112° C., ca. 0.1 mbar) is collected. Yield: 1.90 g.

1. temperaturethe mixture is heated
2. temperatureat reflux for 3 h
3. customThe toluene is evaporated
4. distillationthe mixture is then purified by distillation under reduced pressure
5. customThe first fraction (ca. 35° C., ca. 0.2 mbar)
6. customThe second fraction (ca. 112° C., ca. 0.1 mbar) is collected