医药级二硫代二苯并噻唑合成工艺-研究

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1、万方数据青岛科技大学研究生学位论文TheSyntheticTechnologyofMedicalGradeof2’2'-dibenzothiazoledisulfdeABSTRACTTheresearchtooktheindustrialMastherawmaterial，adoptingtheacidandalkalimethodtopurification，adoptingthegreenoxidant—hydrogenperoxide，usingthenontoxicandlownoxiousorganicreagent，theone—stepmethodsynthesizedthe

2、high—qualityDM．Theproductcouldimmediatelymeettherequestinmedicineproduction，thetechnologywasfeasible．ThestructureoftheproductwascharacterizedusingFT-IRand‘H-NMRtechnology,thepurityoftheproductwascharacterizedusingthemeltingpointapparatusandHPLC．Theproductwasmeasuredbulkdensity．111eorganicreagentwa

3、srecycledtomakesurethewholeprocesswaslowcostandcleanly．ThemethodwasestablishedandstudiedtomeasurethecontentofM．Thefactorsontheresultofacid—alkalimethodMpurificationsuchasthedosageofdeionizedwater,thedosageof32％NaOH，thedosageofactivatedcarbon，thetimeofadsorptionetc．alwereinvestigated，theorthogonale

4、xperimentalandreproducibilityexperimentalweredesigned．TheresultsshowedthatwhenV(deionizedwater)：m(M)=5mL／g，V(32％NaOH)：m(M)=0．6mL／g，m(activatedcarbon)：m(M)21：20，thetimeofadsorptionwas1．5h，theproductwithhighmolecularweightwasobtained．Underthatconditions，theappearanceofproductwaswhitepowder,theyieldo

5、fproductwas97％，theinitialmeltingpointofproductwas1760C，thepurityoftheproductwas98％．ThefactorsontheresultofsolventmethodMpurificationsuchasthedosageofdeionizedwater,thedosageof32％NaOH，thedosageofactivatedcarbon，thetimeofadsorptionetc．alwereinvestigated，theorthogonalexperimentalandreproducibilityexp

6、erimentalweredesigned．TheresultsshowedthatwhenV(deionizedwater)：m∽)210mL／g，V(32％NaoH)：m(M)=0。75mL／g，re(activatedcarbon)：m(M)21：20，thetimeofadsorptionwas3．0h，theproductwithhighmolecularweightwasobtained．Underthatconditions，theappearanceofproductwaswhitepowder,theyieldofproductwas96％，theinitialmelti

7、ngpointofproductwas176。C，thepurityoftheproductwas98％．ThemethodwasestablishedandstudiedtomeasurethecontentofM．TheIII万方数据医药级二硫代为苯并噻唑合成工艺研究resultsshowedth,tattheexcesssodiumsulfitetriplehasfullysatisfiedtherequireme