9,9-Bis(4-aminophenyl)fluorene synthesis

6synthesis methods

Product Name:9,9-Bis(4-aminophenyl)fluorene
CAS Number:15499-84-0
Molecular formula:C25H20N2
Molecular Weight:348.44

9,9-bis(4-aminophenyl)fluorene be used for preparation of high-strength material and high-temperature polymers. 9,9-bis(4-aminophenyl)fluorene can be synthesized in 8 steps from reaction of 9-fluorenone, aniline hydrochloride and sodium bisulfite in toluene 125 - 150℃，followed by experimental steps of stirring, drying, adding filtering etc. to obtain this product.

486-25-9 Synthesis

486-25-9
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62-53-3 Synthesis

62-53-3
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15499-84-0
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$10.00/10g

Yield:15499-84-0 93.4%

Reaction Conditions:

with sodium hydrogen sulphite in toluene at 125 - 150; for 6 h;Temperature;Solvent;

Steps:

3 Example 3

72 g of 9-fluorenone , 155.4 g of aniline hydrochloride, 10 g of sodium bisulfite, and 72 g of a 9-fluorenone, were added to the reaction apparatus equipped with a water trap.145 g of aniline and 100 g of toluene are heated to 125-130° C. under stirring, and incubated at 125-130° C. for 3 hours, and the generated water passes through. Toluene was brought to the trap. Then, the temperature was raised slowly to 145-150 for 3 hours. After the reaction is over, cool down to 95°C. At this temperature, 10% sodium hydroxide solution was added dropwise until the pH of the feed solution was approximately , 95° C., and the mixture was neutralized for 3 hours. Thermal stratification was performed at 95° C., the aqueous layer was separated, and the upper oil layer was collected and added to the flask. Under stirring, the temperature was gradually lowered to 20 to 30°C, and the mixture was sufficiently stirred at 20 to 30°C for 1 hour to be sufficiently crystallized. filter,About 185.6g after drying. 185.6 g of 9,9-bis(4-aminophenyl)fluorene and 300 g of xylene were added to the biscuit, 20 to 30Fully beaten at °C, filter,The product had a wet weight of 170 g, 141 g after drying, and a purity of 99.5% (HPLC normalized content).Obtained above was 141 g of 9,9-bis(4-aminophenyl)fluorene, 2800 g of deionized water, 49.3 g of 33% hydrochloric acid and 28 g ofActivated carbon was added to the flask, and the temperature was raised to 65-70°C to defocus for 2 hours. Heat filtration at 70°C. Add filtrate to burnIn the bottle, add 10% ammonia water and feed solution at pH 60 to 65°C to pH 9 to 10. Stir at 60-65°C for 3 hours.Make it fully neutralized. After the end of the neutralization,After cooling down to 20 to 30°C, filtering and drying the 130g product, the yield is 93.4%, the appearance is pure white solid,The purity is 99.7%.

References:

CN107892649,2018,A Location in patent:Paragraph 0023-0042

486-25-9 Synthesis

486-25-9
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$5.00/25g