A kind of synthetic method of fenbufen
A synthesis method and compound technology, applied in chemical instruments and methods, drug combinations, pharmaceutical formulations, etc., can solve the problems of low product yield, complicated post-treatment purification process, and many synthesis steps, and achieve reaction and post-treatment purification process  Simple, regioselective and high yield, solve the effect of too many steps
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Embodiment 1
[0023] (1) Under an inert atmosphere, mix 0.01mmol allylpalladium(II) chloride dimer, 0.2mmol 2-(dicyclohexylphosphono)-1-phenyl-1H-pyrrole, 1mmol N-(octa Aminoquinoline) but-3-enamide, 5mmol lithium acetate, 3mmol 4-bromobiphenyl, 3mmol cyanoacetic acid, and 100mmol water were mixed, and 0.1mmol of the mixed material and 1mL of anhydrous 2,3-butanediol were added to the reaction vessel Mix well in the medium, place the reaction vessel in an oil bath at 125°C and stir vigorously for 12 hours, and purify the reaction product through a silica gel column (flushing the chromatography silica gel column with petroleum ether at a ratio of ethyl acetate 1:20), to obtain Group compounds;
[0024] (2) 1 mmol of the compound is added to 50 mmol of ethanol solvent containing 1.5 mmol of sodium hydroxide, and the mixture is heated to 130° C. for reflux for 12 hours, and the reaction product is distilled under reduced pressure (the pressure of the reduced pressure distillation is within 100...
Embodiment 2
[0028] (1) Under an inert atmosphere, mix 0.1mmol allylpalladium(II) chloride dimer, 0.02mmol 2-(dicyclohexylphosphono)-1-phenyl-1H-pyrrole, 1mmol N-(octa Aminoquinoline) but-3-enamide, 1mmol lithium acetate, 1)mmol 4-bromobiphenyl, 1mmol cyanoacetic acid and 1mmol water were mixed, and 0.1mmol mixed material and 1mL anhydrous 2,3-butanediol were added to Mix well in the reaction vessel, place the reaction vessel in an oil bath at 125°C and vigorously stir the reaction for 12 hours, and purify the reaction product through a silica gel column (flush the chromatographic silica gel column with petroleum ether at a ratio of ethyl acetate 1:20), to obtain Compounds with directing groups;
[0029] (2) 1mmol of the compound is added to 5mmol ethanol solvent containing 4mmol sodium hydroxide, and the mixture is heated to 140°C for 12 hours under reflux, and the reaction product is subjected to underpressure distillation (the pressure of underpressure distillation is within 100mbar, th...
Embodiment 3
[0033] (1) Under an inert atmosphere, mix 0.05mmol allylpalladium(II) chloride dimer, 0.1mmol 2-(dicyclohexylphosphono)-1-phenyl-1H-pyrrole, 1mmol N-(octa Aminoquinoline) but-3-enamide, 3mmol lithium acetate, 2mmol 4-bromobiphenyl, 2mmol cyanoacetic acid, and 50mmol water were mixed, and 0.1mmol of the mixed material and 1mL of anhydrous 2,3-butanediol were added to the reaction vessel Mix well in the medium, place the reaction vessel in an oil bath at 125°C and stir vigorously for 12 hours, and purify the reaction product through a silica gel column (flushing the chromatography silica gel column with petroleum ether at a ratio of ethyl acetate 1:20), to obtain Group compounds;
[0034] (2) 1 mmol of the compound is added to 30 mmol of ethanol solvent containing 2.5 mmol of sodium hydroxide, and the mixture is heated to 135° C. for reflux for 12 hours, and the reaction product is subjected to underpressure distillation (the pressure of underpressure distillation is within 100 ...
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