发明名称 METHOD FOR SYNTHESIS OF 2-ACETOXY-5-BIPHENYL CARBOXYLIC ACID
摘要 FIELD: chemistry. ^ SUBSTANCE: invention relates to an improved method for synthesis of 2-acetoxy-5-biphenylcarboxylic acid, involving alkylation by adding p-cresol and an alkylation agent into molten pyrophosphoric acid, heating and holding at temperature while stirring, separation of the hydrocarbon layer, washing to a neutral reaction, drying with calcium chloride and rectification under vacuum of 9-10 mm Hg and temperature 151-156C to obtain 4-methyl-2-cyclohexylphenol and then its dehydrogenation in liquid phase at atmospheric pressure and high temperature on palladium catalysts, with extraction of 5-methyl-2-biphenylol when cooling. Alkylation is carried out at 110-120C. The alkylation agent used is cyclohexane. Dehydrogenation is carried out at 300-350C using palladium catalysts in form of palladium catalysts on carbon. After extraction, the 5-methyl-2-biphenylol is acylated in acetic anhydride in the presence of sulphuric acid to 2-acetoxy-5-methylbiphenyl, with subsequent oxidation of the 2-acetoxy-5-methylbiphenyl in a solution of a mixture of glacial acetic acid and acetic anhydride (1:1) with oxygen at temperature 105-110C in the presence of a soluble cobalt-manganese-bromine catalyst until complete oxidation and extraction of 2-acetoxy-5-biphenylcarboxylic acid crystals from the reaction mixture after cooling. ^ EFFECT: method increases output of the valuable 2-acetoxy-5-biphenylcarboxylic acid monomer and lowers the cost of the process. ^ 2 ex
申请公布号 RU2409553(C2) 申请公布日期 2011.01.20
申请号 RU20090102761 申请日期 2009.01.28
申请人 GOSUDARSTVENNOE OBRAZOVATEL'NOE UCHREZHDENIE VYSSHEGO PROFESSIONAL'NOGO OBRAZOVANIJA "JAROSLAVSKIJ GOSUDARSTVENNYJ TEKHNICHESKIJ UNIVERSITET" 发明人 LEBEDEVA NINA VALENTINOVNA;POSTNOVA MARINA VIKTOROVNA;KOSHEL' SERGEJ GEORGIEVICH;KUZNETSOVA ELENA ALEKSANDROVNA;KUKUSHKINA NADEZHDA DMITRIEVNA;JUN'KOVA TAT'JANA ALEKSANDROVNA;LOZINSKAJA OL'GA VLADIMIROVNA;KOSHEL' GEORGIJ NIKOLAEVICH
分类号 C07C67/29;C07C67/52;C07C69/157 主分类号 C07C67/29
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