2-硝基间苯二酚制备工艺的优化

3220045()JOURNALOFHUAIYINTEACHERSCOLLEGE(NATURALSCIENCEEDITION)Vol13No12May.20042-硝基间苯二酚制备工艺的优化韦长梅(,223300):介绍了2-硝基间苯二酚的应用,研究了制备2-硝基间苯二酚的优化工艺.22.00g间苯二酚与60.00g硫酸发生磺化反应,然后与52.00g混酸(含HNO30.28mol,w(HNO3):w(HAc):w(H2SO4)=1g:0.5g:0.5g)在5~10e进行硝化反应6h,再用水蒸汽蒸馏出2-硝基间苯二酚14.96g,总收率48.27%.:间苯二酚;磺化;定向硝化;2-硝基间苯二酚:TQ246.1:A:1671-6876(2004)02-0135-04:2004-01-20:(01KJB150009);(SJ2001019):(1963-),,,,,.02-,,:2-,pH=5.4~7.4,pKIn=6.4?0.1,pT=6.2,pK(pI=7.0),,2-(pKIn=8.3)(pKIn=4.2)[1];2-[24];[5];P-2-HIV-1-[68].,2-[9]:1,,,,12.9%;2,,4,6,37.5%.2,,,6,48.27%,210%.1.12-11.1.AVARTE360FT-IR(Nicolet,),KBr;XT-4(),;Perkin-Elmer240C(Perkin-Elmer,).1.21.2.1磺化250mL22.00g(0.2mol)60.00g(0.6mol),60~65e,3h,3h,.1.2.2硝化-,5e,52.00g(HNO30.28mol,w(HNO3):w(HAc):w(H2SO4)=1g:0.5g:0.5g),5~10e;(2h),2h80g40.00g,1h.1.2.3纯化500mL,,2-14.96g,48.26%.22.12-:82~83e([10]:84~85e).(C9H8N2O1,(),w(C)):46.46(46.51)%;w(H):3.25(3.29)%;w(N):9.03(8.94)%.IR,Mmax:3250~3080cm-1(O-HC-H);1630cm-1,1480cm-1();1560cm-1,1350cm-1(NO2);1250cm-1(C-O).2.2()(w(HNO3):w(HAc):w(H2SO4)=1g:0.5g:0.5g)22.00g(0.2mol),60.00g,44.48g(HNO30.24mol),()5.0h,2-,1.1/(e)-10~-5-5~00~55~1010~15/(g)9.9010.2711.4311.6610.89/(%)31.9433.1236.8737.6235.121:2-,0~10e,5~10e.2.3()(w(HNO3):w(HAc):w(H2SO4)=1g:0.5g:0.5g)22.00g(0.2mol),60.00g,44.48g(HNO30.24mol),5~10e,2-,2.2/(h)4.05.05.56.06.57.0/(g)10.2811.6612.4513.4013.5913.70/(%)33.1737.6240.1543.2243.8544.182,,6h,,136()3,6h.2.4()22.00g(0.2mol),60.00g,5~10e,6h,(w(HNO3):w(HAc):w(H2SO4)=1g:0.5g:0.5g)2-,3.3/(mol)0.20.240.280.300.32/(g)11.3013.4014.9615.0714.87/(%)36.4543.2248.2648.6047.973,,0.28~0.32mol.,0.28mol(n():n()=1.4)26.00g(52.00g).2.5,()(w(HNO3):w(HAc):w(H2SO4)=1g:0.5g:0.5g)22.00g(0.2mol),60.00g,52.00g(HNO30.28mol),5~10e,6h,6(4)2-48.27%.4123456/(g)15.0414.9615.0014.8714.9214.9914.96/(%)48.5248.2648.4047.9748.1348.3648.273:()22.00g(0.2mol),60.00g,52.00g(0.28mol,w(HNO3):w(HAc):w(H2SO4)=1g:0.5g:0.5g),5~10e,6h,2-14.96g,48.27%.462,2-,.:[1]SarwarM,RashidA,ZaidiS.Anewacidbaseindicator:ItspKaandpTvalues[J].PakJSciIndRes,1997,20(1):5759.[2]RoseD,LieskeE,HoeffkesH.Oxidativehairdyescontainingnitrobenzenecouplingagents[P].GerOffen:DE4011481A1,1991-10-10.[3]ManiehA,SayedAZ.Preparationofnewaciddyesfromtoluenederivativesandstudyoftheirdyeingpropertiesonwool[J].A-lAzharBullSci,1995,6(1):3548.[4]ManiehA,SayedAZ.Somenewdyesfrom4-methy-laniline-3-sulfone-2-toluidine[J].A-lAzharBullSci,1995,6(1):4960.[5]AndoKYagiharaM,NaruseH.Processingofcolorphotographicmaterialswithdevelopingbathfreeofbenzylalcohol[P].Jpn:KokaiTokkyoKohoJP63044656A2,1988-02-25.[6]RichardsTP,HamiltonAD.P-Acceptormacrocycles:newcrownetherscontainingisocyanidegroups[J].JChemSocChemCommun,1985(17):11981199.[7],,.2.--1.,3.-[J].,1985,6(1):4548.[8]SaariWS,WaiJS,FisherTE,etal.Synthesisandeveluationof2-pyridinonderivativesasHIV-1-specificreversetranscriptaseinhibitorsAnalogsof3-aminopyridin-2(1H)-one[J].JMedChem,1992,35(21):3792802.[9],,,.[J].,1997,12(2):5962.[10]CadoganJIG,LeySV,PattendenG,etal.DictionaryofOrganicCompounds.SixthEdition[M].London:PublishedbyChapman&Hall,1996.1372:2-OptimizingthePreparationProcessfor2-NitroresorcinolWEIChang-mei(DepartmentofChemistry,HuaiyinTeachersCollege,Huaian223001,China)Abstract:Theapplicationof2-nitroresorcinolwasintroduced.Theoptimizationofprocessforpreparation2-nitro-resorcinolwasstudy.22.00gResorcinolwassulfonatedby60.00gH2SO4andnitratedby52.00gmixtureacid[w(HNO3):w(HAc):w(H2SO4)=1g:0.5g:0.5g]for6hat5~10eandthendistilledbywatervapourtogive14.96g2-nitroresrcinolwithtotalyieldof48.27%.Keywords:resorcinol;sulfonate;orientationnitration;2-nitroresrcinol[:](上接第130页)TheoreticalStudiesontheElectronicStructureandRelatedChemicalPropertiesoftheComplexRu(bpy)2(SCN)2ZHANGYu(DepartmentofChemistry,HuaiyinTeachersCollege,Huaian223001,China)Abstract:TheoreticalstudiesofthecomplexRu(bpy)2(SCN)2wereperformedbyusingRHF/LanL2DZmethod.Thecoordinationbonds,electronicstructure,spectroscopicproperties,andotherrelatedchemicalpropertiesarein-vestigated.Theresultsobtainedmaybeusefulasreferencesforthesynthesisofthecomplexesandthemechanismanalysisonphotochemistryandphotophysics.Keywords:electronicstructure;RuCpolypyridinecomplexes;abinitio[:]138()3