반응 #216029

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 26 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
   기타The temperature of reaction mixture
9. 9
   온도was increased to 110° C.
10. 10
    기타(overnight)
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 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.

출처