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Studies On The Clean Synthesis Of Sucrose Derivatives Sucralose

Posted on:2015-12-09Degree:MasterType:Thesis
Country:ChinaCandidate:C LiFull Text:PDF
GTID:2191330461997281Subject:chemical engineering
Abstract/Summary:PDF Full Text Request
Sucralose as a high quality super sweet functional sweetener, has gradually entered people’s daily lives. Adding a small amount of sucralose in a number of functional drinks, you can achieve the same equivalent of 600 times the sweetness of sucrose general, and not absorbed by the body, which gives a lot of sugar but do not want to bring the gospel to people who dare to eat and such other sugar sweeteners actually no metallic taste,So comprehensive in terms of, is now the best sweetener. Research is focused on the following three aspects of this work:1. Single functional groups protection to trimethylorthoacetate as raw material to the synthesis of sucrose-6-ester can handle special location 6-hydroxyl. This’paper introduces a special acid catalyst. Studied under different conditions will toluenesulfonic load on different substances, through comparison and contrast test, p-toluenesulfonic acid load was measured in polystyrene above can achieve good results, such materials can achieve better catalytic effect of acid, and after filtration and can be reused after catalysis, when up to 5 times the number of repetitions gradually lost catalytic effect. Can not solve the problem of the recovery of p-toluenesulfonic acid. Subsequent hydrolysis step, into sucrose 6-acetate and sucrose-4-acetate, and then to catalytic terbuthylazine amine functional group and a target migration intermediate sucrose-6-acetate.2. The chlorination of sucrose ester is a critical step in the preparation of sucralose, the preparation process is often generated In the above step without purification of sucrose-6-acetate, so the sucrose 6-Crystallization Purification very acetate less paper in the literature of different conditions crystalline sugars reached a sucrose-6-specific programs acetate crystals, the approach is a two-solvent to dissolve sucrose-6-acetate, evaporated low boiling point allow higher boiling poor solvent to dissolve the intermediate and the flow conditions in the crystallization by adding 12 alkylbenzene sulfonate surfactant, bounce, and crystallized.3. Sucralose-6-chlorination process acetate is a key step in this most studied abroad. Mature technology advantages and disadvantages, but the basic principles are the programmed temperature chlorination, temperature control is very important. In this paper, Vilsmeier reagent sucrose 6-acetate selective chloride, and sucrose-6-the molar ratio of acetate (10:1), DMF (ml) and sucrose 6-acetate (g) the ratio (12:1) and reaction time (3h). Sucralose-6-yl acetate prepared by deacetylation of sucralose Recrystallization sucralose-6-acetate in CH3ONa/CH3OH alcoholysis system, with H+ type cation exchange resin, methanol was distilled off, ethyl acetate, etc., decolorized with activated carbon in an aqueous phase, the aqueous solution was concentrated, in the crystallization of hours above 38 ℃, was isolated sucralose. Ethyl acetate and water and recrystallized sucralose can be more than 98% purity sucralose products. The products sucralose, by melting point, IR and H-NMR confirmed the structure.
Keywords/Search Tags:trimethylorthoacetate, sucrose esters, Vilsmeier reagent, programmed temperature, sucralose
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