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Study On The Synthesis Technology Of Sucralose

Posted on:2014-02-17Degree:MasterType:Thesis
Country:ChinaCandidate:J LiFull Text:PDF
GTID:2181330422468511Subject:Chemistry
Abstract/Summary:PDF Full Text Request
In this paper, the synthesis method and process of sucralose were used asfollowing work:The sucrose-6-monoesters were synthesized from sucrose and differentesterifying agent such as methyl benzoate, ethyl acetate, vinyl acetate and trimethylorthoacetate with different catalysts. We get the optimal synthesis method throughexperiments: the sucrose-6-benzoate was synthesized from sucrose and methylbenzoate using cesium carbonate as catalyst. It was investigated that the influence ofthe catalyst dosage, reaction temperature, reaction time and material ratio. Theoptimal reactant conditions were: using cesium carbonate as catalyst with a massfraction of2%based on the mass of sucrose, the molar ratio n(sucrose): n(methylbenzoate)=1:4, the reaction temperature45℃, the vacuum degree0.05MPa, and thereaction time5hours. Under the optimal reaction conditions, the yield ofsucrose-6-benzoate was81.0%.Selective chlorination of the sucrose-6-monoesters is also a key step in thesynthesis of sucralose. In this experiment, firstly vilsmeier reagent was produced bythe reaction of SOCl2and DMF, and then the chlorination reaction was carried outthrough sucrose-6-benzoate/DMF was dropped into the vilsmeier reagent. It wasinvestigated that the influence of different factors. The optimal reactant conditionswere: the reaction temperature110℃, the molar ratio n(SOCl2):n(sucrose-6-benzoate)=8:1, the ratio DMF(mL):sucrose-6-benzoate(g)=10:1, and thereaction time5hours. Ethyl acetate is the extraction agent. Under this condition, theyield of sucralose-6-benzoate was60.2%.In the solution of sodium methoxide/methanol,92.3%sucralose-6-benzoate canbe converted to sucralose under the conditions of10°C and pH=9. The crude productof sucralose was recrystallized twice from water to give pure sucralose. Through thesethree steps, the total yield of sucralose was39.2%.
Keywords/Search Tags:sucralose, sucrose-6-benzoate, cesium carbonate, thionyl chloride
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