Potassium Carbonate → HCID 22023797, compound

HRID 2417010Notes

Reaction equation

HRID 2417010 reaction equation
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:17]2[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=2)([C:13]([F:16])([F:15])[F:14])[C:9]([F:12])([F:11])[F:10])=[CH:4][CH:3]=1.CN(C)[C:26](=O)[CH3:27].[C:30](=[O:33])([O-])[O-].[K+].[K+].[Cl:36][C:37]1[CH:51]=[CH:50][C:40]([C:41]([C:43]2[CH:48]=[CH:47][C:46](F)=[CH:45][CH:44]=2)=[O:42])=[CH:39][CH:38]=1>C1(C)C=CC=CC=1.O>[Cl:36][C:37]1[CH:51]=[CH:50][C:40]([C:41]([C:43]2[CH:48]=[CH:47][C:46]([O:1][C:2]3[CH:7]=[CH:6][C:5]([C:8]([C:17]4[CH:18]=[CH:19][C:20]([O:23][C:48]5[CH:47]=[CH:46][C:45]([C:30](=[O:33])[C:27]6[CH:26]=[CH:51][C:37]([Cl:36])=[CH:38][CH:39]=6)=[CH:44][CH:43]=5)=[CH:21][CH:22]=4)([C:9]([F:10])([F:11])[F:12])[C:13]([F:14])([F:15])[F:16])=[CH:4][CH:3]=3)=[CH:45][CH:44]=2)=[O:42])=[CH:39][CH:38]=1

Participants

7

Reactant 4

HCID 11430Potassium CarbonateHCID 31374DimethylacetamideHCID 73864bisphenol AFHCID 13813634(4-Chlorophenyl)(4-fluorophenyl)methanone

Product 1

HCID 22023797HCID 22023797, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 1140TolueneSolvent2×

Conditions

Temperature
130 °C

Procedure

33.6 g (100 mmol) of 2,2-bis(4-hydroxyphenyl)-1,1,1,3,3,3-hexafluoropropane (bisphenol AF) was measured out in a 11 three-necked flask equipped with an agitator, a Dean-stark tube, a condenser, a three-way cock and a thermometer. The air in the flask was then replaced by dried nitrogen. To the content of the flask were then added 150 ml of N,N-dimethylacetamide and 75 ml of toluene. The mixture was then stirred for dissolution. To the solution was then added 30.4 g (220 mmol) of potassium carbonate. The mixture was then heated to a temperature of 130° C. under reflux. While the resulting water was being boiled together with toluene and removed to the exterior through the Dean-Stark trap, the reaction temperature was then gradually raised to 150° C. After about 1 hour, when most of toluene was removed, the reaction solution was then cooled to a temperature of from 80° C. to 90° C. Subsequently, to the reaction solution was added 58.7 g (250 mmol) of 4-chloro-4′-fluorobenzophenone. The reaction solution was then reacted at a temperature of from 115° C. to 120° C. for 7 hours.

Workup

  1. customequipped with an agitator, a Dean-stark tube, a condenser
  2. temperatureunder reflux
  3. customremoved to the exterior through the Dean-Stark trap
  4. temperaturethe reaction temperature was then gradually raised to 150° C
  5. customwhen most of toluene was removed
  6. temperaturethe reaction solution was then cooled to a temperature of from 80° C. to 90° C
  7. customThe reaction solution was then reacted at a temperature of from 115° C. to 120° C. for 7 hours

Sources & evidence

ORD record
ord-0e1bd4853bdc456eabf5373bc4117811
Source dataset
uspto-grants-2004_11
Patent number
US06825310B2

Reaction notes

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