反应详情

3-(2-Bromotetrafluoroethoxy)-N-(4-(2-bromotetrafluoroethoxy)phenyl)phthalimide Into a 250 ml round bottomed flask fitted with a mechanical stirrer and a Dean-Stark trap is placed 4-(2-bromotetrafluoroethoxy)aniline (3.4 g, 0.0118 mole) in 40 ml of N-methylpyrrolidinone (NMP). In a separate flask, 3-(2-bromotetrafluoroethoxy)phthalic anhydride (3.0 g, 0.00874 mole) is dissolved in 20 ml of NMP and is added slowly drop wise over 15 minutes to the stirring solution of 4-(2-bromotetrafluoroethoxy)aniline in NMP. The mixture is stirred for 30 minutes at room temperature, after which m-xylene (6 ml) is added and the suspension is heated to 40° C. After heating at 40° C. for 1 hour the is heated to reflux (181° C.) and is refluxed for 6.5 hours to remove water azeotropically. Upon cooling the solvent is removed by evaporation under vacuum and the solid precipitate is recrystallized from dichloromethane/hexane solution (2:1) to provide the product as a light yellow crystalline solid (4.37 g, 81.5 percent yield) with a melting point of 172°-172.5° C.

1. temperaturethe suspension is heated to 40° C
2. temperatureAfter heating at 40° C. for 1 hour the
3. temperatureis heated
4. temperatureto reflux (181° C.)
5. temperatureis refluxed for 6.5 hours
6. customto remove water azeotropically
7. temperatureUpon cooling the solvent
8. customis removed by evaporation under vacuum
9. customthe solid precipitate is recrystallized from dichloromethane/hexane solution (2:1)