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Chlorination method for industrial production of sucralose-6-acetate

A technology of sucralose and acetate, applied in chemical instruments and methods, esterified saccharides, sugar derivatives, etc., can solve the problem of increasing raw material costs and solvent recovery workload, high requirements for production process equipment, and prolonging process Process and other issues, to achieve the effect of reducing the separation burden, reducing energy consumption, and speeding up the process

Inactive Publication Date: 2015-06-10
LIYANG WEIXIN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

First of all, the syrup used in this process is dry solid syrup. When chlorinating, N,N-dimethylformamide must be added to dissolve and homogenize. This not only requires high production process equipment, but also greatly increases the cost of raw materials and solvent recovery. workload
Secondly, the dropwise addition of thionyl chloride and syrup before chlorination requires low temperature, which not only prolongs the process, but also requires high equipment and increases energy consumption.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 211g (1.7735mol) of thionyl chloride to 600mL (6.454mol) of trichloroethane below 30°C, then dropwise add 0.2mol of sucrose-6-acetate (water content 0.8%), keep warm after dropping Stir for 0.5 hours, start to heat up, raise the temperature to 80°C in 1 hour, and keep it at 80~90°C for 1 hour; then take 1 hour to raise the temperature to 100°C, and keep it at 100-~105°C for 1 hour; then use The temperature was raised to 110°C in 1 hour, and the temperature was kept at 110~113°C for 1 hour; after the reaction was completed, 45g of the crude product of sucralose-6-acetate was obtained through neutralization, desolventization, decolorization, crystallization, etc., the yield 30%.

Embodiment 2

[0020] Add 211g (1.7735mol) of thionyl chloride to 600mL (6.454mol) of trichloroethane below 25°C, then dropwise add 0.2mol of sucrose-6-acetate (water content 0.5%), keep warm after the addition Stir for 0.5 hours, start to heat up, raise the temperature to 85°C in 1 hour, and keep it at 85~90°C for 1.1 hours; The temperature was raised to 110°C within 1 hour, and kept at 110~113°C for 1.1 hours; after the reaction was completed, 50 g of the crude product of sucralose-6-acetate was obtained through neutralization, desolventization, decolorization, crystallization, etc., and the yield was 34%.

Embodiment 3

[0022] Add 211g (1.7735mol) of thionyl chloride to 600mL (6.454mol) of trichloroethane below 25°C, then dropwise add 0.2mol of sucrose-6-acetate (water content 0.3%), keep warm after dropping Stir for 0.5 hours, start to heat up, raise the temperature to 88°C in 1.1 hours, and keep it at 88~90°C for 1 hour; The temperature was raised to 110°C within 1 hour, and the temperature was kept at 110~113°C for 1 hour; after the reaction was completed, 52 g of the crude product of sucralose-6-acetate was obtained through neutralization, desolventization, decolorization, crystallization, etc., and the yield was 35.46%.

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PUM

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Abstract

A chlorination method for industrial production of sucralose-6-acetate. The method comprises steps of: (a) adding thionyl chloride into an organic solvent below 30 DEG C to form a mixed solution, with a molar ratio of the organic solvent to thionyl chloride of 3.5-4.6:1; (b) adding sucrose-6-acetate with water content of 0.2%-0.8% into the mixed solution, and stirring, wherein a molar ratio of added sucrose-6-acetate to thionyl chloride is 1:7-9; and (c) slowly heating to 110-113 DEG C in 6-7 h; and after the reaction, subjecting the reaction product to neutralization, solvent removal, decolorization by adding water and crystallization to obtain the sucralose-6-acetate crude product. According to the invention, sucrose-6-acetate containing water is adopted for chlorination, and thionyl chloride is added once without cooling, so as to speed up the process, and reduce energy consumption. The employed solvent is more conducive to release of gas products such as sulfur dioxide generated in the chlorination process and promotion of yield increase, and reduces the generation of the other salts and separation burden.

Description

Technical field [0001] The present invention involves the preparation method of trichloro-6-ethyl acetate, which specifically involves the chloride method of industrialized production of three-acetate-6-ethyl acetate. Background technique [0002] Sucralose is a type of chlorine sucrose and is a new type of sweetener.Its sweetness is 650 times that of sucrose. It does not participate in human metabolism, has high safety, has strong acid hydrolysis ability, and has the closest to sucrose among all sweeteners. These advantages make it a preferred product in the market.Siriner-6-ethyl acetate is the key intermediate of the production process of trichloro sucrose.There are usually two types of chloride reagents reported by literature: one is VilSmeier chloride (USP 4980463), and the other is chloribal / pyridine chlorine chloride trifle (USP 5136031).Most of the domestic trichloropa production companies use the first type of Vilsmeier chloride reagent as a chloride reaction raw materia...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H13/06C07H1/00
Inventor 丁红辉蒋朝明刘华
Owner LIYANG WEIXIN CHEM
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