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Catalytic chlorination preparation method of sucralose-6-acetate

A technology of sucralose and acetate, which is applied to the preparation of sugar derivatives, chemical instruments and methods, esterified saccharides, etc., can solve the problems of low product yield and many side reactions, and reduce production costs. The effect of reducing three wastes, increasing efficiency, saving energy, reducing emission and reducing consumption

Pending Publication Date: 2022-02-18
ANHUI JINGHE IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the problem of many side reactions and low product yield in the reaction process, and to provide a catalytic chlorination of sucralose-6-acetate in view of the deficiency of the technical scheme in the patent publication number CN 102070678B. Preparation method; on the basis of the reaction system described in the patent publication number CN 102070678B, the present invention adds the catalyst described in the present invention to it, catalyzes the chlorination reaction, and suppresses the occurrence of side reactions, thereby improving the sucralose-6- Acetate yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Thionyl chloride was used as the chlorination agent to investigate the reaction effects of various catalysts:

[0026] Get 150 mL of trichloroethane, add the chlorination catalyst as shown in Table 1, add 26 mL of thionyl chloride under stirring conditions, add 45 mL of DMF solution of 30% sucrose-6-acetate dropwise while stirring under ice-water bath conditions, Keep warm for 1 hour; transfer the reaction device to an oil bath heating, heat up to 45°C, keep warm for 1 hour; heat up to 70°C, keep warm for 2 hours; heat up to 90°C, keep warm for 1 hour; heat up to 100°C, keep warm for 1.5 hours; Raise the temperature to 114°C and keep it warm for 2 hours; transfer the reaction device to an empty water bath device, use ice water to cool down to 0-5°C, add dropwise 20% ammonia water to neutralize to PH = 9, react with hydrochloric acid for 1 hour Adjust the pH to 7; evaporate the solvent in vacuum, add water three times to entrain and evaporate DMF with high boiling point,...

Embodiment 2

[0030] Using solid phosgene as a chlorinating agent, the reaction effects of various catalysts were investigated:

[0031] Take 150 mL of trichloroethane, add 30 g of solid phosgene under stirring conditions, after the dissolution is complete, add the chlorination catalyst as shown in Table 1, and add DMF with a concentration of 30% sucrose-6-acetate dropwise while stirring under ice-water bath conditions Solution 45mL, keep warm for 1 hour; transfer the reaction device to an oil bath heating, heat up to 40°C, keep hold for 1 hour; heat up to 70°C, keep hold for 2 hours; heat up to 90°C, keep hold for 1 hour; 1.5 hours; heat up to 114°C, keep warm for 2 hours; transfer the reaction device to an empty water bath device, use ice water to cool down to 0-5°C, add dropwise 20% ammonia water to neutralize to pH = 9, and react for 1 hour Finally, adjust the pH to 7 with hydrochloric acid; evaporate the solvent in vacuum, add water three times to entrain and steam out high-boiling DMF...

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Abstract

The invention relates to a catalytic chlorination preparation method of sucralose-6-acetate, which comprises the existing preparation steps and is characterized in that a chlorination catalyst accounting for 0.0001-6% of the weight of a chlorinating agent is added in the preparation process. The method has the advantages that the chlorinating agent is used for catalyzing the chlorination reaction, side reaction can be inhibited, tar carbonization is reduced, follow-up treatment is simple, the yield of sucralose-6-acetate is increased to 65-85% from original 55-75%, the production cost is reduced, three wastes are reduced, and therefore remarkable effects on efficiency improvement, energy conservation, emission reduction and consumption reduction are achieved.

Description

technical field [0001] The invention belongs to the technical field of sucralose production and relates to a catalytic chlorination preparation method of sucralose-6-acetate. Background technique [0002] Sucralose (TGS), a new type of sweetener jointly developed by Tate & Lyle and the University of London and applied for a patent in 1976; it is the only functional sweetener with sucrose as raw material, the original brand name For Splenda, it is 600 times sweeter than sucrose. This sweetener has the characteristics of no energy, high sweetness, pure sweetness, and high safety. It is one of the best functional sweeteners at present. [0003] The industrial production of sucralose adopts the monoester method, using DMF as the solvent, acetic anhydride as the acylating agent to obtain sucrose-6-acetate, usually using thionyl chloride as the chlorinating agent for chlorination to obtain three Sucralose-6-acetate, then alcoholysis to produce sucralose. [0004] The chlorinati...

Claims

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Application Information

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IPC IPC(8): C07H13/04C07H1/00
CPCC07H13/04C07H1/00
Inventor 周睿肖世东陈永旭陈朝晖张正颂
Owner ANHUI JINGHE IND
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