Synthesis method of 4-cyclopentyl biphenyl fluorinated compound
A technology of cyclopentyl biphenyl and cyclopentenyl biphenyl is applied in the field of synthesizing fluorine-containing compounds of 4-cyclopentyl biphenyl, and can solve the problem of low yield of fluorine-containing compound IX, high environmental protection pressure and shortened service life of facilities and other problems, to achieve the effect of convenient post-processing, high safety performance, and low environmental pollution.
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Embodiment 1
[0018] Example 1, a synthesis method of 4-cyclopentylbiphenyl fluorine-containing compound IX, this embodiment is a synthesis method of 4'-cyclopentyl-3,5-difluorobiphenyl, the synthesis route is as follows:
[0019]
[0020]
[0021] Wherein the preparation of 4-cyclopentenyl chlorobenzene V is: under the protection of inert gas, in the 500ml reaction bottle that mechanical stirring, reflux condensation drying tube, feeding funnel are housed, add magnesium sheet 13g, THF35ml successively, stir; To 50°C, add dropwise 20ml of the prepared p-chlorobromobenzene 100g / THF100ml mixed solution into the system, the reaction is initiated, and the temperature is controlled at 50°C to 70°C to add dropwise. A good cyclopentanone 50g / toluene 200ml mixed solution, stop the reaction 90min after the dropwise addition, pour the reaction solution into a 500ml reaction bottle with 100ml of concentrated hydrochloric acid, stir for 2h, then add 100ml of toluene, stir for 1h and let it stand ...
Embodiment 2
[0025] Example 2, a synthesis method of 4-cyclopentylbiphenyl fluorine-containing compound IX, this embodiment is a synthesis method of 4'-cyclopentyl-3,4,5-trifluorobiphenyl, the synthesis route is as follows:
[0026]
[0027] Wherein the preparation of 4-cyclopentenyl chlorobenzene V is: under the protection of inert gas, in the 500ml reaction bottle that mechanical stirring, reflux condensation drying tube, feeding funnel are housed, add magnesium sheet 13g, THF35ml successively, stir; To 70°C, add dropwise 20ml of the prepared p-dichlorobenzene 77g / THF100ml mixed solution into the system, the reaction is initiated, and the temperature is controlled at 70°C to 80°C to add dropwise. A good cyclopentanone 50g / toluene 200ml mixed solution, 120min after the dropwise addition, stop the reaction, pour the reaction solution into a 500ml reaction bottle with 100ml of concentrated hydrochloric acid, stir for 2h, then add 100ml of toluene, stir for 1h and let it stand Separate th...
Embodiment 3
[0031] Embodiment 3, a synthetic method of 4-cyclopentylbiphenyl fluorine-containing compound IX, this embodiment is a synthetic method of 4'-cyclopentyl-3-fluorobiphenyl, the synthetic route is as follows:
[0032]
[0033] Wherein the preparation of 4-cyclopentenyl chlorobenzene V is: under the protection of inert gas, in the 500ml reaction bottle that mechanical stirring, reflux condensation drying tube, feeding funnel are housed, add magnesium sheet 13g, THF35ml successively, stir; To 70°C, add dropwise 20ml of the prepared p-chloroiodobenzene 125g / THF100ml mixed solution into the system, the reaction is initiated, and the temperature is controlled at 40°C to 50°C to add dropwise. A good cyclopentanone 50g / toluene 200ml mixed solution, 120min after the dropwise addition, stop the reaction, pour the reaction solution into a 500ml reaction bottle with 100ml of concentrated hydrochloric acid, stir for 2h, then add 100ml of toluene, stir for 1h and let it stand Separate the...
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