Method for synthesizing 4-cyclobutyl biphenyl fluorine-containing compound
A technology of cyclobutyl biphenyl and cyclobutenyl biphenyl is applied in the field of synthesis of 4-cyclobutyl biphenyl fluorine-containing compounds, and can solve the problems of high risk factor, high pressure on environmental protection, large amount of waste water and the like, and achieve safety The effect of high performance, less environmental pollution and less operation steps
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Embodiment 1
[0017] Example 1, a synthesis method of 4-cyclobutylbiphenyl fluorine-containing compound IX, this embodiment is a synthesis method of 4'-cyclobutyl-3,5-difluorobiphenyl, the synthesis route is as follows:
[0018]
[0019]
[0020] Wherein the preparation of 4-cyclobutenyl 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 cyclobutanone 47g / toluene 200ml mixed solution, 90min 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 Sep...
Embodiment 2
[0024] Example 2, a synthesis method of 4-cyclobutylbiphenyl fluorine-containing compound IX. This example is a synthesis method of 4'-cyclobutyl-3,4,5-trifluorobiphenyl. The synthesis route is as follows:
[0025]
[0026]
[0027] Wherein the preparation of 4-cyclobutenyl 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 cyclobutanone 47g / toluene 200ml mixed solution, stop the reaction 120min 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 Separat...
Embodiment 3
[0031] Embodiment 3, a synthetic method of 4-cyclobutylbiphenyl fluorine-containing compound IX, this embodiment is a synthetic method of 4'-cyclobutyl-3-fluorobiphenyl, the synthetic route is as follows:
[0032]
[0033] Wherein the preparation of 4-cyclobutenyl 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 cyclobutanone 47g / toluene 200ml mixed solution, stop the reaction 120min 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 Separate the liqu...
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