Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 627871-16-3, name is 5-Bromo-4-fluoro-2-methylaniline, A new synthetic method of this compound is introduced below., Quality Control of 5-Bromo-4-fluoro-2-methylaniline
470 g of 5-bromo-4-fluoro-2-methylaniline (2.30 mol, 1.0 eq), 667 g of 2-bromocyclopropyl ketone (3.68 mol, 1.6 eq), organic solvent were added to the reaction flask. And alkali reagent, organic reagent is 3L toluene, alkali reagent is 623gDiisopropylamine ethylamine (4.83 mol, 2.1 eq), heated to 110 C for 12 hours, TLC detection showed the reaction was completed (PE / EA = 10/1, product Rf = 0.6, PE is petroleum ether, EA is Ethyl acetate). After the reaction: the mixture was cooled to room temperature, 1.5 liters of water and 1.5 liters of ethyl acetate were added, and the organic phase was separated with saturated ammonium chloride solution (500 mL), saturated sodium hydrogen carbonate solution (500 mL), and brine (500 mL) Wash once, dry anhydrous sodium sulfate (60g), spin dry, use 2L petroleum ether / acetic acidEthyl ester = 15/1 mixed solvent is beaten to obtain a solid product486 g (1.70 mol) of 2-(5′-bromo-4′-fluoro-2′-methylphenyl)amino-1-cyclopropyl ketone in a yield of 75%.
The synthetic route of 627871-16-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Douchuang (Shanghai) Pharmaceutical Technology Co., Ltd.; Wang Lei; Xu Zhi; Wang Zongying; Chen Da; Fu Haixiang; Li Ming; Ai Youqing; (11 pag.)CN109608441; (2019); A;,
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