ChemicalBook CAS DataBase List 2,2-Bis(3-amino-4-hydroxyphenyl)hexafluoropropane

2,2-Bis(3-amino-4-hydroxyphenyl)hexafluoropropane synthesis

6synthesis methods

Product Name:2,2-Bis(3-amino-4-hydroxyphenyl)hexafluoropropane
CAS Number:83558-87-6
Molecular formula:C15H12F6N2O2
Molecular Weight:366.26

2,2-Bis(3-amino-4-hydroxyphenyl)hexafluoropropane (6FAP) is a useful research chemical as white crystals. 6FAP can be synthesized from Fluorobenzene as a starting material through a four-step reaction.

Phenol, 4,4'-[2,2,2-trifluoro-1-(trifluoromethyl)ethylidene]bis[2-nitro-

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2,2-Bis(3-amino-4-hydroxyphenyl)hexafluoropropane

83558-87-6
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Yield:83558-87-6 98.3%

Reaction Conditions:

with palladium-carbon;hydrogen in N,N-dimethyl-formamide at 70; under 7500.75 Torr;Autoclave;

Steps:

7; 5-6 The preparation steps include

Put 30g of bis(3-nitro-4-hydroxyphenyl)hexafluoropropane into a 1000mL autoclave,Add 300g DMF and 1.5g palladium/carbon (the mass fraction of palladium in palladium/carbon is 5%),Press the hydrogen gas to 1MPa, turn on the stirring and raise the temperature to 70,Stop the reaction when the content of bis(3-nitro-4-hydroxyphenyl)hexafluoropropane is less than 0.1%,The target product bis(3-amino-4-hydroxyphenyl)hexafluoropropane gas content is 98%,The system is black. The temperature of the kettle is lowered to room temperature, filtered, and the filtrate is dried under reduced pressure at 70-80°C to obtain crude bis(3-amino-4-hydroxyphenyl)hexafluoropropane. The crude product is recrystallized.The recrystallization solvent is water and DMF, bis(3-amino-4-hydroxyphenyl)hexafluoropropane,The mass ratio of water and DMF is 1:4:2. First mix the crude bis(3-nitro-4-hydroxyphenyl)hexafluoropropane with the recrystallization solvent and raise the temperature of the kettle to 60°C and stir,Then the kettle temperature was lowered to 10-20°C for crystallization, filtered and dried to obtain 25.4g of pure bis(3-nitro-4-hydroxyphenyl)hexafluoropropane.The yield of bis(3-amino-4-hydroxyphenyl)hexafluoropropane was 98.3%, and the purity was 99.6%.

References:

CN111302944,2020,A Location in patent:Paragraph 0116-0122; 0131-0134