Adding a certain compound to certain chemical reactions, such as: 384-16-7, name is 2-Bromo-1-chloro-3-(trifluoromethyl)benzene, belongs to chlorides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 384-16-7, Formula: C7H3BrClF3
Under nitrogen substitution,2-Bromo-3-chlorobenzotrifluoride (212 mg)Of tetrahydrofuran (0.7 mL)Was added isopropyl magnesium chloride / lithium chloride complex / tetrahydrofuran solution (1.3 M, 0.63 mL) dropwise at room temperature and stirred for 1 hour.This solution was added to the ice-cooled compound (172 mg) obtained in Example 46c,In diethyl ether (3 mL) over 5 minutes.Thereafter, the mixture was stirred under ice-cooling for 2 hours and at room temperature for 2.5 hours.Since the reaction was not completed,Again 2-bromo-3-chlorobenzotrifluoride (212 mg),From isopropyl magnesium chloride / lithium chloride complex / tetrahydrofuran solution (1.3 M, 0.63 mL)Grignard reagent was prepared by the same operation as above,Was added dropwise to the ice-cooled reaction solution over 5 minutes.After stirring for 1 hour under ice cooling, 0.5N hydrochloric acid was added and the mixture was extracted with ethyl acetate.The extract layer was washed successively with water, saturated aqueous sodium hydrogen carbonate solution and saturated brine,After drying with anhydrous sodium sulfate and filtration, the solvent was distilled off under reduced pressure.The obtained residue was purified by silica gel column chromatography (ethyl acetate / hexane) to obtain the title compound (71.0 mg) as a colorless transparent gummy solid.
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Reference:
Patent; DAIICHI SANKYO COMPANY LIMITED; NAGAMOCHI, MASATOSHI; KOZAWA, YUJI; INAGAKI, HIROAKI; GOTANDA, KENTOKU; NOGUCHI, TETSUJI; TORIHATA, MUNEFUMI; YOSHINO, TOSHIHARU; ISOBE, TAKASHI; (113 pag.)JP2016/141632; (2016); A;,
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