In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 1603-41-4 as follows., 1603-41-4
Water (20 mL),3-Chloro-4- (4-methylphenyl) -4-oxobutanoic acid(5.02 g, 0.022 mol),2-Amino-5-methylpyridine (3) (3.58 g, 0.033 mol)And sodium carbonate (2.33 g, 0.022 mol) were successively added to a 100 mL reaction flask,After mixing,Slowly warmed to 80 internal temperature, nitrogen protection,Insulation reaction 7h, 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 0.1g, 50 decolorization 30min, hot filtration,The filtrate was adjusted to pH = 3.0 ~ 3.5 with 6N aqueous sodium hydroxide solution to precipitate a solid,Cooling to 0 ~ 5 insulation 1h, suction filtration, the filter cake with 10mL ice water rinse,80 vacuum drying 6h,3.21 g of pale yellow solid (HPLC: 97.6%) was obtained in a yield of 52.0%.
The chemical industry reduces the impact on the environment during synthesis 1603-41-4, I believe this compound will play a more active role in future production and life.
Reference:
Patent; East China University of Science and Technology; Zhao Jianhong; Guan Yu; Liao Fan; Deng Weiping; Shi Xiaoxin; Zhao Jinyuan; Ma Lirong; Chen Chunyan; Yang Jun; Li Jie; Lei Qingyun; (11 pag.)CN107383005; (2017); A;,
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