반응 #216030

반응 방정식

potassium carbonate

4,4'-difluorobenzophenone

dimethylacetamide

4-nitrophthalonitrile

→

phthalonitrile

용매

water

Water

Toluene

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 light pink reaction mixture was stirred at 90° C. for 1 hour
4. 4
   온도The reaction mixture was refluxed at 145°-150° C. for 10 hours
5. 5
   기타was removed by azeotropic distillation
6. 6
   기타The toluene was removed by distillation
7. 7
   온도Upon cooling to room temperature
8. 8
   기타The temperature of reaction mixture
9. 9
   온도was increased to 70° C.
10. 10
    기타(overnight)
11. 11
    온도The temperature was further increased to 110° C.
12. 12
    workup.WAITheld for 1 hour
13. 13
    workup.STIRRINGwith stirring
14. 14
    여과The solid precipitate was collected by suction filtration
15. 15
    세척washed exhaustively with water
16. 16
    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 (36.7 mmol) of bisphenol A6F, and 40 ml of dimethylacetamide (DMAC). 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 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 10 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 room temperature, 6.37 gm (36.8 mmol) of 4-nitrophthalonitrile was added. The temperature of reaction mixture was increased to 70° C. and held at this temperature for 16 hours (overnight). The temperature was further increased to 110° C. and held for 1 hour. The room temperature mixture was poured into 400 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 16.9 gm of oligomeric phthalonitrile monomer.

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