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Method for preparing sucralose-6-acetate

A technology of sucralose and acetate, applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of high reaction temperature requirements, increased difficulty in operation, long reaction time, etc., and achieve the goal of "three wastes" Less, convenient post-processing, and simple process operation

Inactive Publication Date: 2015-02-18
SUZHOU JONATHAN NEW MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The difficulty of this process lies in the second step of chlorination reaction. Most domestic processes use DMF as solvent, and chlorinated reagents are used for chlorination. The reaction temperature is high and the reaction time is long. Due to the generation of hydrogen chloride and sulfur dioxide gas during the reaction, if it cannot be timely and effective Excluding it will lead to carbonization of the product, and the operation will increase

Method used

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  • Method for preparing sucralose-6-acetate
  • Method for preparing sucralose-6-acetate

Examples

Experimental program
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Embodiment 1

[0023] Preparation of Sulfonated Cage Mesoporous Carbon

[0024] Using F127 as the structure-directing agent and tetraethyl orthosilicate as the silicon source, after hydrothermal synthesis at 150°C, the structure-directing agent was calcined in a muffle furnace to obtain mesoporous silica KIT-5-150, which is characterized by ordered mesoporous Silicon KIT-5-150 is the silicon template, sucrose is the carbon source, and the sucrose is repeatedly poured into the silicon template twice, after thermal polymerization, a mesoscopic phase is formed, and then carbonized in a nitrogen atmosphere, and finally the silicon template is soaked in hydrofluoric acid , to obtain cage-type mesoporous carbon CKT-3 (A); CKT-3 (A), isoamyl nitrite and p-aminobenzenesulfonic acid were added to water, at 80 ° C and under stirring, with isoamyl nitrite and The sulfonic acid phenyl radical generated by the reaction of p-aminobenzenesulfonic acid reacted with the mesoporous carbon CKT-3(A) to achieve ...

Embodiment 2

[0030] The difference between this example and Example 1 lies in the preparation of the phthalate-based cationic gemini surfactant.

[0031] In 250 milliliters of three-necked round bottom flasks, add respectively dimethyl phthalate 58g (0.03mol), N, N-dimethylethanolamine 11g (0.12mol), the sulfonated bamboo charcoal catalyst 10g that embodiment 2 makes, The reaction was heated at 100°C for 5 hours, and methanol was continuously distilled out from the system. After 12 hours, it was changed to vacuum distillation to recover excess N,N-dimethylethanolamine. Cool to room temperature, add 60 ml of chlorohexane, reflux and stir for 24 hours, distill off the solvent, cool and solidify, and recrystallize from acetonitrile to obtain the product.

Embodiment 3

[0033] The difference between this example and Example 1 lies in the preparation of the phthalate-based cationic gemini surfactant.

[0034] In 250 milliliters of three-necked round bottom flasks, add respectively dimethyl phthalate 58g (0.03mol), N, N-dimethylethanolamine 11g (0.12mol), the sulfonated bamboo charcoal catalyst 10g that embodiment 3 makes, The reaction was heated at 100°C for 5 hours, and methanol was continuously distilled out from the system. After 12 hours, it was changed to vacuum distillation to recover excess N,N-dimethylethanolamine. Cool to room temperature, add 60 ml of benzyl chloride, reflux and stir for 24 hours, distill off the solvent, cool and solidify, and recrystallize from acetonitrile to obtain the product.

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Abstract

The invention discloses a method for preparing sucralose-6-acetate. The method comprises the following steps: adding saccharose, trimethyl orthoacetate and a sulfonated cage type mesoporous carbon catalyst into a reaction container for C-6 hydroxyl protective reaction of saccharose; after reaction, adding a phthalate cation dimeric surfactant shown in a formula (I) for chlorination; after reaction, extracting by using ethyl acetate; decoloring by using active carbon; and concentrating and crystallizing to obtain a sucralose-6-acetate product, wherein in the formula (I), R is C1-C10 alkyl, allyl or benzyl. The method has the characteristics of simple process operation, good technical performance, few three wastes and reusable reaction system, is convenient for post-treatment and is an environmental friendly technology which is economic and practical.

Description

technical field [0001] The invention relates to a method for preparing sucralose-6-acetate. Background technique [0002] Sucralose is also called sucralose, TGS for short, and its chemical name is 4,1',6'-trichloro-4,1',6'-trideoxygalactosucrose. It is a white powder product and is very soluble. In water, the solubility in water at 20°C is 28.2g / dL. It has high chemical stability in acidic solution, and after long-term (10 years) rigorous tests on pharmacology, toxicology, physiology, physiology and chemistry, it has been proved that sucralose is harmful to humans. safe. Because of its pure sweetness, it is very similar to the natural product sucrose, which is 600 times sweeter than sucrose, and has no unpleasant aftertaste brought by other sweeteners; it is not absorbed by the human body, does not produce heat, and does not interact with insulin when metabolized. It can be eaten by diabetics, obese patients and the elderly; it will not cause caries and is helpful to dent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H13/06C07H1/00
Inventor 李卓才李苏杨
Owner SUZHOU JONATHAN NEW MATERIALS TECH