반응 #216031

반응 방정식

4-nitrophthalonitrile

potassium carbonate

4,4'-difluorobenzophenone

dimethylacetamide

→

phthalonitrile

용매

Toluene

Water

water

반응 조건

후처리

1. 1
   기타To a 100 ml, 3-necked flask equipped with a thermometer
2. 2
   workup.ADDITIONwas added
3. 3
   workup.STIRRINGThe reaction mixture was stirred at 70° C. for 1 hour
4. 4
   온도The reaction mixture was refluxed at 145°-150° C. for 24 hours
5. 5
   기타was removed by azeotropic distillation
6. 6
   기타The toluene was removed by distillation
7. 7
   온도Upon cooling to 50° C.
8. 8
   온도the temperature of the mixture was increased to 110° C.
9. 9
   기타(overnight)
10. 10
    workup.STIRRINGwith stirring
11. 11
    여과The solid precipitate was collected by suction filtration
12. 12
    세척washed exhaustively with water
13. 13
    기타dried

실험 절차

To a 100 ml, 3-necked flask equipped with a thermometer and a Dean-Stark trap was added 5.0 gm (22.9 mmol) of 4,4'-difluorobenzophenone, 8.03 gm (23.9 mmol) of bisphenol A6F, and 50 ml of dimethylacetamide (DMAC). After flushing the mixture for 30 minutes with dry nitrogen, 3.9 gm (28.7 mmol) of pulverized anhydrous potassium carbonate was added with stirring. The reaction mixture was stirred at 70° 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 24 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., 3.10 gm (17.9 mmol) of 4-nitrophthalonitrile was added. Since the reaction mixture was somewhat viscous, the temperature of the mixture was increased to 110° C. and held at this temperature for 18 hours (overnight). FTIR spectroscopy showed the absence of hydroxy and nitro bands. The room temperature mixture was then poured into 300 ml of water with stirring to break the precipitate into a powdery form. The solid precipitate was collected by suction filtration, washed exhaustively with water, and dried to afford 11.5 gm of oligomeric phthalonitrile monomer.

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