A kind of synthetic method of pharmaceutical intermediate diaryl substituted pyridine derivative
A synthetic method and pyridine technology, applied in the synthesis of 2,6-diaryl substituted pyridine derivatives and the synthesis of pyridine derivatives, achieving good application prospects and wide industrial production potential
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Embodiment 1
[0042]
[0043]In an appropriate amount of organic solvent 1,4-dioxane, add 100mmol of the above formula (I) compound, 200mmol of the above formula (II) compound, 5mmol catalyst (for 1.6mmol PdCl 2 (cod) and 3.4mmol p-toluenesulfonate nickel mixture), 10mmol phosphine ligand L1, 50mmol base DMPA and 10mmol accelerator (a mixture of 2mmol ferrocene and 8mmol cobalt nitrate), then heated to 60 ° C, and in The reaction was stirred well at this temperature for 10 hours.
[0044] After the reaction was finished, filter to obtain the filtrate, add a 10% hydrochloric acid aqueous solution to the filtrate, adjust the pH value to 6-7, then fully shake and extract with ethyl acetate for 2-3 times, combine the organic phases, and remove Pressure distillation concentrated, the residue was separated by 200-300 mesh silica gel column chromatography (eluted with a mixture of ethyl acetate and chloroform with a volume ratio of 1:2), so as to obtain the compound of formula (III), the yield ...
Embodiment 2
[0048]
[0049] In an appropriate amount of organic solvent 1,4-dioxane, add 100mmol of the above formula (I) compound, 250mmol of the above formula (II) compound, 7mmol catalyst (for 2mmol PdCl 2 (cod) and 5mmol p-toluenesulfonate nickel mixture), 12mmol phosphine ligand L1, 60mmol base DMPA and 15mmol accelerator (a mixture of 3mmol ferrocene and 12mmol cobalt nitrate), then heated to 70 ° C, and in the The reaction was stirred well at temperature for 8 hours.
[0050] After the reaction was finished, filter to obtain the filtrate, add a 10% hydrochloric acid aqueous solution to the filtrate, adjust the pH value to 6-7, then fully shake and extract with ethyl acetate for 2-3 times, combine the organic phases, and remove Pressure distillation concentrated, the residue was separated by 200-300 mesh silica gel column chromatography (eluted with a mixture of ethyl acetate and chloroform with a volume ratio of 1:2), so as to obtain the compound of formula (III), the yield was...
Embodiment 3
[0054]
[0055] In an appropriate amount of organic solvent 1,4-dioxane, add 100mmol of the above formula (I) compound, 300mmol of the above formula (II) compound, 9mmol catalyst (for 2.25mmol PdCl 2 (cod) and 6.75mmol p-toluenesulfonate nickel mixture), 15mmol phosphine ligand L1, 80mmol base DMPA and 20mmol accelerator (a mixture of 4mmol ferrocene and 16mmol cobalt nitrate), then heated to 80 ° C, and in The reaction was stirred well at this temperature for 7 hours.
[0056] After the reaction was finished, filter to obtain the filtrate, add a 10% hydrochloric acid aqueous solution to the filtrate, adjust the pH value to 6-7, then fully shake and extract with ethyl acetate for 2-3 times, combine the organic phases, and remove Pressure distillation concentrated, the residue was separated by 200-300 mesh silica gel column chromatography (eluted with a mixture of ethyl acetate and chloroform with a volume ratio of 1:2), so as to obtain the compound of formula (III), the yie...
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