Process for producing 2,2-bis[3-amido-4-(4-aminophenoxy)phenyl] hexafluoropropane
A technology of aminophenoxy and hexafluoropropane, applied in 2 fields, can solve the problems such as no patents, literature reports and the like in the preparation method, and achieve the effects of convenient source of raw materials, high yield and few chemical raw materials
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[0026] Example 1
[0027] Mix 60.8 grams (0.1 mole) of 2,2-)bis[3-amino-4-(4-nitrophenoxy)phenyl]hexafluoropropane, 0.7 grams of palladium with a mass percentage of 15% palladium on carbon, 250 Milliliter ethanol and 670ml ethylene glycol were added to the reaction flask, stirred, heated to 60°C, and started to add dropwise a 60% mass concentration hydrazine hydrate solution (hydrazine hydrate molecular weight 50.06), a total of 208.3 grams (solution weight). After the dropwise addition of hydrazine hydrate is completed, continue to stir and react for 1 hour in the temperature range of 70°C to 85°C, cool slightly, filter while hot, cool the mother liquor, add an appropriate amount of pure water dropwise to precipitate the crystalline product, filter, and vacuum dry to obtain 51.1 G 2,2-bis[3-amino-4-(4-aminophenoxy)phenyl]hexafluoropropane crystals with a purity of 99.6%. According to the actual 2,2-bis[3-amino-4- (4-Aminophenoxy)phenyl]hexafluoropro...
Example Embodiment
[0028] Example 2
[0029] Mix 60.8 grams (0.1 mol) of 2,2-bis[3-amino-4-(4-nitrophenoxy)phenyl]hexafluoropropane, 12.1 grams of palladium / carbon with 1% palladium mass percentage and 6000ml ethanol Add it into the reaction flask, stir, heat and increase the temperature to 60°C, and start to add dropwise a hydrazine hydrate solution with a mass concentration of 85%, a total of 47.1 grams (solution weight). After the dropwise addition of hydrazine hydrate is completed, continue to stir and react for 5 hours in the temperature range of 70°C to 85°C, cool slightly, filter while hot, cool the mother liquor, add an appropriate amount of pure water dropwise, precipitate the crystalline product, filter, and dry in vacuum to obtain 36.8 G 2,2-bis[3-amino-4-(4-aminophenoxy)phenyl]hexafluoropropane crystals with a purity of 99.0%. According to the actual 2,2-bis[3-amino-4- (4-Aminophenoxy)phenyl]hexafluoropropane amount and theoretical amount (54.8g), calculated to...
Example Embodiment
[0030] Example 3
[0031] Mix 60.8 grams (0.1 mol) of 2,2-bis[3-amino-4-(4-nitrophenoxy)phenyl]hexafluoropropane, 4.0 grams of palladium / carbon with a palladium mass percentage of 5% and 1500ml 2 -Methoxyethanol was added to the reaction flask, stirred, heated to 60°C, and started to add hydrazine hydrate solution with a mass concentration of 80%, a total of 130.0 grams (solution weight). After the dropwise addition of hydrazine hydrate is completed, continue to stir and react for 4 hours in the temperature range of 70°C to 85°C, cool slightly, filter while hot, cool the mother liquor, add an appropriate amount of pure water dropwise, precipitate the crystalline product, filter, and vacuum dry to obtain 51.3 G 2,2-bis[3-amino-4-(4-aminophenoxy)phenyl]hexafluoropropane crystals with a purity of 99.7%. According to the actual 2,2-bis[3-amino-4- (4-Aminophenoxy)phenyl]hexafluoropropane amount and theoretical amount (54.8g), calculated to obtain 2,2-bis[3-am...
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