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With ammonium hydroxide; sodium tetrahydroborate; 10 wt% Pd(OH)2 on carbon; In 5,5-dimethyl-1,3-cyclohexadiene; at 150℃; for 36h;Inert atmosphere;
Put a moderate stirrer in a dry reaction tube (20 ml), add palladium hydroxide / carbon (20 mol%),NaBH4 (2 times equivalent), then the reaction tube is evacuated, filled with argon, repeated three times, dissolved in an argon atmosphereA solution of <strong>[330-93-8]bis(4-fluorophenyl)ether</strong> (0.2 mmol) and aqueous ammonia (1 mmol) in xylene was slowly added to the reaction tube with a syringe, which was reversed.The tube should be placed in a 150 C oil bath and heated and stirred. After 36 hours, the reaction was stopped and the reaction tube was taken out of the oil bath.It was naturally cooled to room temperature, diluted with ethyl acetate, and then the reaction liquid was filtered with celite, and the yield of the filtrate was determined by gas phase detection.62%. The filtrate was concentrated and separated by an activated thin layer chromatography chromatography plate (eluent: n-hexane/ethyl acetate = 30/1).The final product 3a is obtained after separation. Product 3a (yield: 48%)
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