Synthesis, Isolation And Characterization Of Sucralose And Its Intermediates

Based on the primary purpose of studying the synthesis,isolation and the characterization of sucralose and its intermediates,and the second purpose of studying the analysis and monitoring methods during the synthesis process of sucralose;The synthesis and purification methods usually introduced in Organic Chemistry were used for guiding ideology in this paper; A better synthesis route was chosen after reading many references,the reaction conditions were further optimized,the impact factors of the yield were discussed.The thin layer chromatography and column chromatography separation conditions of sucralose and its intermediates that sucrose-6-ester and sucralose-6-ester were successfully found,high purity products of sucralose and its intermediates were made after the purification,the structure of sucralose and it's intermediates was identified by IR and MS,the purity was determined by HPLC.(1) Designed a synthesis route,in which sucrose was used as the starting raw materials, dibutyltin oxide as the catalyst to synthetize sucrose -6 - ester,then SOCl₂,DMF and ethyl acetate were used to chlorinate the sucrose-6-ester to produce a sucralose-6-ester,at last NaOCH₃ was used as the catalyst deacylate the sucralose-6-ester in methanol solution to synthetize sucralose.The advance of the process line lied in many aspects:it's easy to operate, the yield was relatively high,the reaction conditions were mild,the raw materials were readily available and relatively inexpensive,the waste was less and easy to be handled,etc.(2) The thin layer chromatography and column chromatography separation conditions of sucralose as well as its intermediates that sucrose-6-ester and sucralose-6-ester were successfully found,high purity products of sucralose and its intermediates that sucrose-6-ester and sucralose-6-ester were made after the purification;The structure of sucralose and it's intermediates was identified by IR and MS,their primary functional groups,molecular weight and molecular structure were also confirmed.A reliable basis was provided for synthetizing the standard production of the intermediates.(3) The optimum conditions of every reaction were discussed,during the chlorination of sucrose-6-ester,the reaction temperature was controlled by adding ethyl acetate which is a low boiling point solvent,the chlorination process in which DMF and SOCl₂ were used as Vilsmeier reagents was improved;The factors impact on yield and decoloured effect were discussed.(4) The conditions of Separating and testifying sucralose and its intermediates using High Performance Liquid Chromatography were initially explored,which provide a reliable reference when promoting the use of High Performance Liquid Chromatography to control the entire synthesis process of sucralose industrial producing(5) The IR and MS of sucralose and its intermediates were researched in detail,the laws of chemical bond fracture were found in IR.