Toluene → bisphenol-Z benzophenone

HRID 1700787

Reaktionsgleichung

Reaktionsgleichung von HRID 1700787
[CH2:1]1[CH2:6][CH2:5][C:4]([C:14]2[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][CH:15]=2)([C:7]2[CH:12]=[CH:11][C:10]([OH:13])=[CH:9][CH:8]=2)[CH2:3][CH2:2]1.C(=O)([O-])[O-].[K+].[K+].F[C:28]1[CH:42]=[CH:41][C:31]([C:32]([C:34]2[CH:39]=[CH:38][C:37](F)=[CH:36][CH:35]=2)=[O:33])=[CH:30][CH:29]=1.C1(C)C=CC=CC=1>O.CN(C)C(=O)C>[CH2:1]1[CH2:6][CH2:5][C:4]([C:7]2[CH:8]=[CH:9][C:10]([OH:13])=[CH:11][CH:12]=2)([C:14]2[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][CH:15]=2)[CH2:3][CH2:2]1.[C:32]([C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1)(=[O:33])[C:31]1[CH:41]=[CH:42][CH:28]=[CH:29][CH:30]=1

Komponenten

7

Edukt 4

HCID 1140TolueneHCID 95824,4'-DifluorobenzophenoneHCID 11430Potassium CarbonateHCID 2324461,1-Bis(4-hydroxyphenyl)cyclohexane

Produkt 1

HCID 131722563bisphenol-Z benzophenone

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×HCID 31374DimethylacetamideLösungsmittel

Versuchsvorschrift

In a three neck 500 mL round-bottom flask was weighed bisphenol-Z (35.0000 g, 130.42 mmol), potassium carbonate (36.0505 g, 260.45 mmol), 4,4′-difluorobenzophenone (28.4587 g, 130.42 mmol), toluene (115 g) and N,N-dimethylacetamide (233 g). The flask was fitted with a condenser and a thermometer. The light yellow mixture was stirred and heated to reflux. The water formed was azeotropically distilled with toluene. On complete removal of water and toluene, the solution was stirred at reflux for about 2 hours. The viscous polymer solution was precipitated in water, and a white fibrous polymer was isolated by filtration. The white polymer was stirred in boiling water for about 1 hour, filtered, and then stirred in boiling methanol for about 1 hour and filtered. The fibrous white polymer was then dried in an vacuum oven for about 16 hours at 100° C. The yield was about 54.35 g. The number average molecular weight of the polymer was about 11.5K.

Aufarbeitung

  1. customThe flask was fitted with a condenser
  2. temperatureheated to reflux
  3. distillationwas azeotropically distilled with toluene
  4. customOn complete removal of water and toluene
  5. stirringthe solution was stirred
  6. temperatureat reflux for about 2 hours
  7. customThe viscous polymer solution was precipitated in water
  8. customa white fibrous polymer was isolated by filtration
  9. stirringThe white polymer was stirred
  10. customfor about 1 hour
  11. filtrationfiltered
  12. stirringstirred
  13. customfor about 1 hour
  14. filtrationfiltered
  15. customThe fibrous white polymer was then dried in an vacuum oven for about 16 hours at 100° C

Quellen und Nachweise

ORD-Eintrag
ord-09a6bfe8bd1041448a30ca8891e83ef9
Quelldatensatz
uspto-grants-2002_02
Patentnummer
US06350553B2

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