Synthesis of 3,4,5-trifluoro-2'-nitro-1,1'-biphenyl

doi:10.16085/j.issn.1000-6613.2015.04.038

Chemical Industry and Engineering Progree ›› 2015, Vol. 34 ›› Issue (04): 1122-1125.DOI: 10.16085/j.issn.1000-6613.2015.04.038

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Synthesis of 3,4,5-trifluoro-2'-nitro-1,1'-biphenyl

LIU Chengxian

Deparmtment of Chemical Engineering, Changzhou Institute of Engineering Technology, Changzhou 213164, Jiangsu, China

Received:2014-12-16 Revised:2015-01-04 Online:2015-04-05 Published:2015-04-05

3,4,5-三氟-2'-硝基联苯的工艺合成

刘承先

常州工程职业技术学院, 江苏常州 213164

作者简介:刘承先,(1963—),男,副教授,主要研究方向为化学工程与工艺.E-mail cxliu@email.czie.net.

Abstract

Abstract: 3,4,5-trifluoro-2'-nitro-1,1-biphenyl was an important intermediate for the synthesis of Fluxapyroxad. It was obtained with 3,4,5-trifluorophenyl boronic acid and 1-chloro-2-nitrobenzene as starting materials,Ms-Pd as the catalyst of coupling reaction. The optimal reaction condition was obtained as reaction temperature of 40℃,and reaction time of 10h,with Ms-Pd as catalyst,DMF as solvent,K₂CO₃ as deacid reagen,1-chloro-2-nitrobenzene and 3,4,5-trifluorophenyl boronic acid as reactants. Under the optimal condition,a yield of 92% was obtained. The product content was 98.3%. Ms-Pd catalyst activity remained after four time recycling.

Key words: 3,4,5-trifluoro-2'-nitro-1,1'-biphenyl, coupling reaction, Ms-Pd

摘要： 3,4,5-三氟-2'-硝基联苯是合成杀菌剂氟唑菌酰胺的重要原料.本文考察了以3,4,5-三氟苯硼酸与邻氯硝基苯为原料,Ms-Pd(分子筛负载氯化钯)作为偶联反应催化剂,制备3,4,5-三氟-2'-硝基联苯.通过反应条件优化,实验确定的最佳反应条件是:以Ms-Pd为催化剂,碳酸钾为缚酸剂, DMF为反应溶剂,邻氯硝基苯和3,4,5-三氟苯硼酸进行反应,反应温度40℃,反应时间10h.产品收率92%,液相含量98.3%.催化剂Ms-Pd套用4次活性无降低.

关键词: 3,4,5-三氟-2'-硝基联苯, 偶联反应, Ms-Pd

CLC Number:

TQ246.1⁺3

LIU Chengxian. Synthesis of 3,4,5-trifluoro-2'-nitro-1,1'-biphenyl[J]. Chemical Industry and Engineering Progree, 2015, 34(04): 1122-1125.

刘承先. 3,4,5-三氟-2'-硝基联苯的工艺合成[J]. 化工进展, 2015, 34(04): 1122-1125.

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Synthesis of 3,4,5-trifluoro-2'-nitro-1,1'-biphenyl

3,4,5-三氟-2'-硝基联苯的工艺合成

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