Reference of 17715-69-4, A common heterocyclic compound, 17715-69-4, name is 1-Bromo-2,4-dimethoxybenzene, molecular formula is C8H9BrO2, 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.
A thermometer, a stirrer, a reflux condenser attached to the flask, and subjected to nitrogen gas purging, 1-bromo-2,4-dimethoxybenzene 110g, 257g IPA, and potassium carbonate added to the solution previously prepared by dissolving 139g to 107g water and the reaction vessel was stirred while nitrogen It is replaced, and then tetrakistriphenylphosphine palladium (0), adding to 5.9g, also 4-methoxy-phenylboronic acid to pre-IPA 109g 83g Solution was added dropwise to the dissolved. After 3 hours the reaction mixture was heated to reflux, added 500mL of water, separate the IPA layer, the water layer was Transferred to a separatory funnel, the toluene extract was added 500mL. An organic layer was washed with saturated sodium chloride solution each. Solvents in vacuo After distilling off the one, added 500mL of toluene, and the precipitate was separated by filtration, toluene was distilled off under reduced pressure. Methane to the obtained crude product Adding to come 200mL, taking over the precipitate, and dried 5 hours in a vacuum dryer of 50 , 2,4,4′- tree fertilization methoxy phenyl Gained 105g
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; Dainippon Inc. & Chemicals; Yoshimoto, Yasuyo; Morinika, Kunihiro; Kinoshita, Hiroshi; (17 pag.)KR2016/8529; (2016); A;,
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