626-43-7, 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 626-43-7 as follows.
Under constant stirring at 0 C, to a solution of 3,5-dichloroaniline (3.24 g, 20 mmol)concentrated hydrochloric acid solution (12 mL)35 wt.% aqueous solution of acetaldehyde (12.8 mL, 80 mmol) was added dropwise. The reaction mixture was stirred at 0 C for 15 minutes and then gradually warmed to 75 C. And reacted at this temperature for 4 hours. The reaction was cooled to room temperature, poured into ice water, 25% aqueous ammonia solution was added dropwise and made alkaline,Extract with dichloromethane three times.The organic phase was separated, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure.The crude product was isolated and purified by silica gel column chromatography (ethyl acetate / petroleum ether, 1: 20) to obtain 2.93 g of the compound 1 as a pale yellow solid in a yield of 69%.
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 626-43-7, and friends who are interested can also refer to it.
Reference:
Patent; Guangdong University of Technology; Centre national de la recherche scientifique (CNRS); LIU, YAN; LIU, XING GUO; HUANG, DA YA; HUANG, MEI JIE; WANG, DE AN; NGUYEN, MICHELLE; ROBERT, ANNIE; MOONEY, BERNARD; (18 pag.)CN105949120; (2016); A;,
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