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ChemicalBook CAS DataBase List 2,2-Bis(4-aminophenyl)hexafluoropropane

2,2-Bis(4-aminophenyl)hexafluoropropane synthesis

4synthesis methods
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Yield:1095-78-9 87.4%

Reaction Conditions:

with guanidine hydrochloride salt;nickel dichloride in ethanol at 85; under 1500.15 Torr;Inert atmosphere;Autoclave;Solvent;Pressure;Temperature;

Steps:

1-3; 1

Weigh 33.6g of bisphenol AF, 1.3g of nickel chloride and 9.5g of guanidine hydrochloride,Put 165g of ethanol in a beaker, mix well and add the reaction system into the autoclave,Replace with nitrogen three times, pressurize to 0.2MPa, turn on stirring,Slowly increase the temperature to 85°C, after the reaction is over, remove the solvent by distillation under reduced pressure,Add 120g water and 150g ethyl acetate, adjust the pH to 7.5 with saturated sodium bicarbonate solution,Separate the liquid to obtain the organic phase, decolorize with activated carbon, and dry with anhydrous sodium sulfate.30.7g of white crude product 2,2-bis(4-aminophenyl)hexafluoropropane was obtained by de-solventization under reduced pressure, with a yield of 92.3%.Purity: 96.7%, ethyl acetate: petroleum ether (volume ratio = 1:3) recrystallized to obtain pure product 29.1g, yield 87.4%,Purity: 99.2% (see the HPLC profile in Figure 1).

References:

CN111302948,2020,A Location in patent:Paragraph 0008; 0021-0033

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