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With sodium carbonate In water at 60℃; for 6 h; Inert atmosphere
Water (100 mL), 3-bromo-4- (4-methylphenyl) -4- oxobutanoic acid (25.12 g, 0.093 mol)2-Amino-5-methylpyridine (3) (10.02 g, 0.093 mol)And sodium carbonate (9.86 g, 0.093 mol) were successively added to a 500 mL reaction flask, After mixing,Slowly warmed to an internal temperature of 60 ° C,Nitrogen protection, thermal reaction 6h,Stop the reaction.With 6N hydrochloric acid pH = 0.5 ~ 1,Stirred at room temperature for 30min,No change in pH after the test, adding an equal amount of ethyl acetate,Stir 15min, points to the reservoir,Water layer plus activated carbon 0.5g, 50 decolorization 30min, hot filtration,The filtrate was adjusted with 6N aqueous sodium hydroxide pH = 3.0 ~ 3.5,Precipitation solid, cooled to 0 ~ 5 insulation 1h, suction filtration,The filter cake was rinsed with 50 mL of ice water and dried under vacuum at 80 ° C. for 6 h.21.38 g (HPLC: 99.2percent) of a light yellow solid was obtained in a yield of 82.0percent.
Reference：
[1] Patent: CN107383005, 2017, A, . Location in patent: Paragraph 0054; 0055-0063; 0070; 0071; 0072-0079
With sodium carbonate; In water; at 60℃; for 6h;Inert atmosphere;
Water (100 mL), 3-bromo-4- (4-methylphenyl) -4- oxobutanoic acid (25.12 g, 0.093 mol)2-Amino-5-methylpyridine (3) (10.02 g, 0.093 mol)And sodium carbonate (9.86 g, 0.093 mol) were successively added to a 500 mL reaction flask, After mixing,Slowly warmed to an internal temperature of 60 C,Nitrogen protection, thermal reaction 6h,Stop the reaction.With 6N hydrochloric acid pH = 0.5 ~ 1,Stirred at room temperature for 30min,No change in pH after the test, adding an equal amount of ethyl acetate,Stir 15min, points to the reservoir,Water layer plus activated carbon 0.5g, 50 decolorization 30min, hot filtration,The filtrate was adjusted with 6N aqueous sodium hydroxide pH = 3.0 ~ 3.5,Precipitation solid, cooled to 0 ~ 5 insulation 1h, suction filtration,The filter cake was rinsed with 50 mL of ice water and dried under vacuum at 80 C. for 6 h.21.38 g (HPLC: 99.2%) of a light yellow solid was obtained in a yield of 82.0%.
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