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METHOD OF PRODUCING 4-METHOXYBIPHENYL BY SUZUKI-MIYAURA REACTION

机译:铃木-宫崎反应制备4-甲氧基苯的方法

摘要

FIELD: chemistry.;SUBSTANCE: invention relates to a method of producing 4-methoxy biphenyl using Suzuki-Miyaura reaction and can be used in chemical and pharmaceutical industries for producing bi-aryls, which are important intermediate products in synthesis of pharmaceutical preparations, ligands and polymers. Method involves reaction of 4-bromanizol and phenylboronic acid in solvent in presence of base and Pd/MN100 synthesized by impregnation of over above cross-linked polystyrene of MN100 grade with precursor, heating reaction mixture in gas atmosphere in molar excess of phenylboronic acid in relation to 4-bromanizol 1.5. At that, for process of impregnation precursor used is solution (CH3CN)2PdCl2 in tetrahydrofurane impregnation is carried out at temperature from 20°C to 40°C, wherein content of palladium in catalyst ranges from 0.5 to 2 wt% using preliminarily milled MN100, amount of catalyst ranges from 0.5 to 1.5 mol% with respect to 4-bromanizol, as reaction solvent mixture of ethanol/water at ratio of 1:0 to 1:2 is used and, as base is NaOH, K2CO3 and Na2CO3 in amount of 1-2 mmol at temperature from 50 to 75°C for 10 min to 1 h in gas atmosphere of nitrogen or air.;EFFECT: proposed method allows to efficiently obtain end product with high technological effectiveness of process.;1 cl, 6 dwg, 7 tbl, 7 ex
机译:用铃木-宫浦反应生产4-甲氧基联苯的方法技术领域本发明涉及一种使用铃木-宫浦反应(Suzuki-Miyaura reaction)生产4-甲氧基联苯的方法,可用于化学和制药工业生产联芳基,联芳基是药物制剂,配体合成中的重要中间产物和聚合物。该方法涉及在碱和Pd / MN100的存在下,通过将以上MN100级的交联聚苯乙烯浸渍到前体中而合成的4-溴苯甲唑和苯基硼酸在溶剂中的反应,在气体气氛中加热摩尔过量苯基硼酸的反应混合物。到4-bromanizol 1.5。在此情况下,所用的浸渍前体是在四氢呋喃中浸渍的溶液(CH 3 CN) 2 PdCl 2 作为乙醇/水的反应溶剂混合物,使用初步研磨的MN100,其中催化剂中钯的含量为0.5至2重量%,相对于4-溴苯甲酚,催化剂的量为0.5至1.5摩尔%,其中比例为1:0到1:2,并且以NaOH为碱,K 2 CO 3 和Na 2 CO 3 的量为1-2 mmol;效果:所提出的方法可高效获得具有高技术效力的最终产品1 cl,6 dwg,7 tbl,7 ex

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