반응 #216033

반응 방정식

4-nitrophthalonitrile

potassium carbonate

4,4'-difluorobenzophenone

N-methyl pyrrolidinone

→

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 100° C. for 1 hour
4. 4
   온도The reaction mixture was refluxed at 175°-180° C. for 12 hours
5. 5
   기타was removed by azeotropic distillation
6. 6
   기타was reduced to 160° C.
7. 7
   기타by removing the glass stopper from the 3-necked flash
8. 8
   기타reached 180° C.
9. 9
   기타had been removed
10. 10
    온도The temperature of the mixture was increased to 100° C.
11. 11
    workup.STIRRINGwith stirring
12. 12
    여과The solid precipitate was collected by suction filtration
13. 13
    세척washed exhaustively with water
14. 14
    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, 11.56 gm (34.4 mmol) of bisphenol A6F, and 80 ml of N-methyl pyrrolidinone (NMP). After flushing the mixture for 30 minutes with dry nitrogen, 7.6 gm (55.1 mmol) of pulverized anhydrous potassium carbonate was added with stirring. The reaction mixture was stirred at 100° 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 175°-180° C. for 12 hours. Water which formed as a by-product was removed by azeotropic distillation. The reaction temperature was reduced to 160° C. and the toluene was sweep out of the reaction vessel by removing the glass stopper from the 3-necked flash. When the temperature reached 180° C., it was assumed that the toluene had been removed. Upon cooling to room temperature, 3.97 gm (22.9 mmol) of 4-nitrophthalonitrile was added. The temperature of the mixture was increased to 100° C. and held at this temperature for 4 hours. FTIR spectroscopy showed the absence of hydroxy and nitro bands. The room temperature mixture was then poured into 400 ml of water with stirring. The solid precipitate was collected by suction filtration, washed exhaustively with water, and dried to afford 9.1 gm of oligomeric phthalonitrile monomer.

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