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间二氯苯合成间氯苯甲醚的工艺研究

DOI: 10.3969/j.issn.1000-2006.2015.05.025

Keywords: 间二氯苯, 甲醇钠, 甲氧基化反应, 间氯苯甲醚
1
, 3-dichlorobenzene, sodium methoxide, methoxylation reaction, m-chloroanisole

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Abstract:

以间二氯苯和甲醇钠为原料,对间氯苯甲醚合成的新工艺进行了研究; 通过单因素实验考察了溶剂种类及用量、间二氯苯与甲醇钠的摩尔比、反应温度、反应时间对间二氯苯转化率和间氯苯甲醚得率的影响,并采用正交实验法对反应条件进行了优化。确定了适宜的合成工艺条件为:以N,N-二甲基甲酰胺(DMF)作溶剂,溶剂用量为75 mL/mol,n(间二氯苯):n(甲醇钠)=1:1.2,反应温度为120 ℃,反应时间6 h。在此工艺条件下,间二氯苯的转化率为94.8%,间氯苯甲醚的得率为91.0%。采用FT-IR和GC-MS分析技术对间氯苯甲醚进行了表征。
A new preparation process for m-chloroanisole was explored from 1,3-dichlorobenzene and sodium methoxide. The effects of types of solvent and their dosage, mole ratio of 1,3-dichlorobenzene to sodium methoxide, reaction temperature and reaction time on the conversion rate of 1,3-dichlorobenzene and yield of m-chloroanisole was examined. The optimum synthesis conditions were obtained by orthogonal test as follows: N, N-dimethyl-formamide(DMF)was used as solvent, and solvent dosage was 75 mL/mol; the molar ratio of 1,3-dichlorobenzene to sodium methoxide was 1:1.2; reaction temperature was 120 ℃ and reaction time was 6 h. Under this optimum conditions, the conversion rate of 1,3-dichlorobenzene was 94.8% and the yield of 1,3-chloroanisole was 91.0%. The structure of the m-chloroanisole was analyzed by FT-IR and GC-MS

References

[1]  flicksk,frankuse,fridtrichse.phenylsubstituiertenaminomethylcyciohexanolen[j].arzneimforsch,1978,28(1):107-114.
[2]  schlosserm,heissc,marzie,etal.protonmobilityin2-substituted1,3-dichlorobenzenes“ortha”or“meta”metalation[j].europeanjournaloforganicchemistry,2006(19):4398-4404.
[3]  schlotterk,boeckerf,huebnerh,etal.fancybioisosteresmetallocene-derivedg-protein-coupledreceptorligandswithsubnanomolarbindingaffinityandnovelselectivityprofiles[j].journalofmedicinalchemistry,2005,48(11):3696-3699.
[4]  maleczkare,shif,holmesd,etal.c―hactivation/borylation/oxidationaone-potunifiedroutetometa-substitutedphenolsbearingortho-para-directinggroups[j].journaloftheamericanchemicalsociety,2003,125(26):7792-7793.
[5]  zilbermanj.one-stepprepartonofsome3-substitutedanisoles[j].organicprocessresearch&development,2003(7):303-305.
[6]  ouks,thiebauds,borredone,etal.o-methylationofphenoliccompoundswithdimethylcarbonateundersolid/liquidphasetransfersystem[j].tetrahedronletters,2002,43(14):2661-2663.
[7]  testaferril,tieccom,tingolim,etal.thereactionsofunactivatedarylhalideswithsodiummethoxideinhmpa[j].tetrahedron,1983,39(1):193-197.
[8]  bogdald,pielichowskij,borona.newsyntheticmethodofaromaticethersundermicrowaveirradiationindrymedie[j].syntheticcommunications,1998,28(16):3029-3039.
[9]  gibsonsp,tommasinii.preparationof4-arylpiperidinesandtheirusefortreatmentofpruritus:jp,2001019672[p].2001-01-23.
[10]  davisjm,favord,faylk,etal.preparationof
[11]  [1,naphthyridin-2-onesandrelatedcompoundsforthetreatmentofschizophrenia,othermentaldisorders,andcentralnervoussystemdisorders:us,2005043309[p].2005-02-24.
[12]  薛建荣,钟宏,符剑刚.碳酸二甲酯的用途及合成研究进展[j].化工技术与开发,2006,35(3):8-13.xuejr,zhongh,fujg.usageofdimethylcarbonateanditssynthesisdevelopment[j].technologyanddevelopmentofchemicalindustry,2006,35(3):8-13.
[13]  langliosb,soulag.asafeandeconomicalsynthesisof3-(trifluoromethoxy)anilinefrom2-chlorophenol[j].bulletindelasocietechimiquedefrance,1986,6:925-929.
[14]  董燕敏,尹振燕,程琦,等.碳酸二甲酯作为甲基化试剂合成2,6-二氯苯甲醚[j].精细化工,2010,27(7):667-671.dongym,yinzy,chengq,etal.synthesisof2,6-dichloroanisolewithdimethylcarbonateasmethylatingagent[j].finechemicals,2010,27(7):667-671.
[15]  陈兴权,刘洋,董燕敏,等.碳酸二甲酯作甲基化试剂合成邻氯苯甲醚[j].精细化工,2008,25(8):817-820.chenxq,liuy,dongym,etal.synthesisofo-chioroanisolewithdimethylcarbonateasmethylatingagent[j].finechemicals,2008,25(8):817-820.
[16]  与善信,文瑞明.相转移催化合成对硝基苯甲醚[j].精细化工,2003,33(5):19-20.yusx,wenrm.thesynthesisofp-nitroanisolebyphasetransfercatalysis[j].finechemicals,2003,33(5):19-20.
[17]  徐晓维,徐徐,王石发,等.甲基丙烯酸异冰片酯的合成及性能研究[j].南京林业大学学报:自然科学版,2013,37(4):133-138.xuxw,xux,wangsf,etal.synthesisandpropertiesofisobornylmethacrylate[j].journalofnanjingforestryuniversity:naturalsciencesedition,2013,37(4):133-138.
[18]  nationalinstituteofstandardsandtechnology.benzene,1-chloro-3-methoxy[eb/ol].http://webbook.nist.gov/cgi/cbook.cgi?id=2845-89-8&units=si.

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