Reference of 16618-68-1, These common heterocyclic compound, 16618-68-1, name is 3-Bromo-5-methoxyaniline, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
In 50 ml by adding three-necked bottle 1.01g3-methoxy-5-bromoaniline(5mmol), 1.40g (5.5mmol) connecting boric acid frequency ester, 1.47g (15mmol) and potassium acetate PdCl2(dppf) catalyst (150 mg), vacuum pumping and nitrogen injection 6 times, the state of the protection of nitrogen by adding DMSO (25 ml), 80 C reaction 18h, in a water cooling retrodisplacement, precipitate after filtering, washing, drying to obtain the crude column chromatography separation (petroleum ether: ethyl acetate = 1:5) shall be 1.03g yellow powdery solid, yield 82.4%.The 0.99g the above-mentioned preparation of the compound (4mmol) by adding 100 ml round-bottom flask, add 30 ml of methanol is dissolved, add 0.56gNH4Cl (10mmol), constant voltage dropping funnel for slowly dripping 2.56gNaIO4(12mmol) of 7 ml aqueous solution, stirring the mixture at room temperature for reaction 18h, TLC detection, filtering to remove the inorganic salt, methanol filters after evaporation to dryness, drying to obtain the crude product purification column chromatography (petroleum ether: ethyl acetate = 1:5) shall be near white powdery solid 0.53g, yield 79.1%.
The synthetic route of 16618-68-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Ocean University of China; Jiang, Tao; Yin, ruijuan; Zhang, Li Juan; (38 pag.)CN103497211; (2016); B;,
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