4,4'-Difluorobenzophenone → Phthalonitrile

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

To a 100 ml, 3-necked flask equipped with a thermometer and a Dean-Stark trap was added 4.0 gm (18.4 mmol) of 4,4'-difluorobenzophenone, 12.33 gm (36.7 mmol) of bisphenol A6F, and 40 ml of dimethylacetamide (DMAC). After flushing the mixture for 30 minutes with dry nitrogen, 10.1 gm (73.4 mmol) of pulverized anhydrous potassium carbonate was added with stirring. The light pink reaction mixture was stirred at 90° C. for 1 hour. Toluene was added to the Dean-Stark trap and to the reaction vessel (4 ml). The reaction mixture was refluxed at 145°-150° C. for 26 hours. Water which formed as a by-product was removed by azeotropic distillation. The toluene was-removed by distillation while heating to 160° C. Upon cooling to 50° C., 6.37 gm (36.8 mmol) of 4-nitrophthalonitrile was added. The reaction mixture was observed to be viscous. The temperature of reaction mixture was increased to 110° C. and held at this temperature for 16 hours (overnight). The room temperature mixture was poured into 200 ml of water with stirring. The solid precipitate was collected by suction filtration, washed exhaustively with water, and dried to afford 20.1 gm of oligomeric phthalonitrile monomer.

Herkunft & Nachweise