Synthesis method of N-biphenyl carbazole
A technology of biphenylcarbazole and synthesis method, applied in the direction of organic chemistry and the like, can solve the problems of complex reaction system, difficult separation and purification, and by-products, etc., and achieves the effects of simple process operation, cheap raw materials, and reduced reaction cost.
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Embodiment 1
[0023] This embodiment provides a kind of synthetic method of N-biphenylcarbazole, and synthetic route is:
[0024]
[0025] The synthesis steps are as follows:
[0026] 17.2 grams of 4-fluorobiphenyl was added to 100 milliliters of dimethyl sulfoxide (DMSO), and then 20 g of carbazole was added to the above solution. Under nitrogen protection, the temperature was lowered to 0 degrees Celsius, and 2.9 g of sodium hydride ( NaH), control the internal temperature not to exceed 25 degrees Celsius, after the addition is complete, stir for 2 hours, then raise the temperature to 120 degrees, stir overnight, and TLC detects that the raw material 4-fluorobiphenyl disappears. Then the reaction solution was slowly poured into 5 liters of stirred water, continued to stir for 2 hours, then suction filtered to obtain a solid, washed with water, and then recrystallized with ethanol / water to obtain 30.5 g of a solid with a purity of 99.8% and a yield of 95.3%.
[0027] The NMR data are: ...
Embodiment 2
[0029] This embodiment provides a kind of synthetic method of N-biphenylcarbazole, and synthetic route is:
[0030]
[0031] The synthesis steps are as follows:
[0032] Add 17.2 grams of 4-fluorobiphenyl to 100 milliliters of dimethyl sulfoxide and 10 milliliters of water, then add 20 grams of carbazole to the above solution, under nitrogen protection, cool down to 0 degrees Celsius, and add 4.8 grams of sodium hydroxide in batches (NaOH) and 2.6g of tetrabutylammonium fluoride, the internal temperature is controlled not to exceed 25 degrees Celsius, after the addition is completed, the temperature is then raised to 140 degrees, stirred overnight, and TLC detects that the raw material 4-fluorobiphenyl disappears. Then the reaction solution was slowly poured into stirred 5 liters of ice water, continued to stir for 2 hours, then suction filtered to obtain a solid, washed with water, and then recrystallized with ethanol / water to obtain 28.6 g of a solid with a purity of 99.6...
Embodiment 3
[0034] This embodiment provides a kind of synthetic method of N-biphenylcarbazole, and synthetic route is:
[0035]
[0036] The synthesis steps are as follows:
[0037] 17.2 grams of 3-fluorobiphenyl was added to 100 milliliters of dimethyl sulfoxide, and then 20 grams of carbazole was added to the above solution. Under nitrogen protection, the temperature was lowered to 0 degrees Celsius, and 2.9 grams of sodium hydride (NaH) was added in batches. Control the inner temperature not to exceed 25 degrees Celsius. After the addition is complete, stir for 2 hours, then raise the temperature to 120 degrees, and stir overnight. TLC detects that the raw material 3-fluorobiphenyl disappears. Then the reaction solution was slowly poured into 5 liters of stirred water, continued to stir for 2 hours, then suction filtered to obtain a solid, washed with water, and then recrystallized with ethanol / water to obtain 29.1 g of a white solid with a purity of 99.8% and a yield of 90.9%. The...
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