反应详情

1.64 m((18 mmol) of phosphorus oxychloride are taken in 10 ml of anhydrous acetonitrile. Under argon, a solution of 1.85 g (16.8 mmol) of 90% strength dimethylaminoacrolein in 7 ml of acetonitrile is first added dropwise at -10° C. to 0° C., and a solution of 1.76 g (6 mmol) of 3-(4-fluorophenyl)-5-isopropyl-1-methyl-2-phenyl-pyrrole (Example 3) in 7 ml of acetonitrile is then added at -5° C. to 0° C. The mixture is heated under reflux overnight. It is now added to a suspension of 4.4 g of sodium hydroxide in 65 ml of water and 65 ml of toluene at 10° C. such that the temperature does not rise above 25° C. After the mixture has been stirred at room temperature for 1.5 hours, it is filtered over kieselguhr and the phases are separated.

1. temperatureThe mixture is heated
2. temperatureunder reflux overnight
3. customdoes not rise above 25° C
4. filtrationit is filtered over kieselguhr
5. customthe phases are separated