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Preparation method of sucralose

A technology of sucralose and sucralose, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of affecting commercial application, long process flow of sucralose, complicated operation, etc., to avoid excessive Effects of chlorination and polymerization reactions, simplified operation steps, and improved reaction efficiency

Inactive Publication Date: 2014-07-02
CHANGMAO BIOLOGICAL LIANYUNGANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process of preparing sucralose by this method is long and complicated, and the use of ionic liquid as a solvent also directly affects the commercial application of the process.

Method used

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  • Preparation method of sucralose

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The preparation method of sucralose comprises the steps:

[0021] (1) Put 150 grams of sucrose (342.3 grams per mole of sucrose) into N,N-dimethylformamide, then add toluenesulfonic acid and trimethyl orthoacetate, keep stirring at 30°C for 8 hours; add water, Stir at 25°C for 2 hours; add tert-butylamine and stir at 20°C for 2 hours; rectify under reduced pressure at 2mmHg and below 50°C to remove water and part of N,N-dimethylformamide to obtain 0.05% water Sucrose-6-acetate N, N-dimethylformamide solution, the mol ratio of described sucrose, N, N-dimethylformamide, toluenesulfonic acid, trimethyl orthoacetate, water, t-butylamine is: 1:22:0.02:1.5:8.0:0.4;

[0022] (2) At 0°C, add benzyltriethylammonium chloride (TEBA) to N,N-dimethylformamide, then add thionyl chloride, mix to obtain a mixture, and keep it warm for 2 hours; Next, add 2,6-di-tert-butyl-p-cresol (BHT) to the mixture, then add the solution obtained in step (1), and keep the reaction for 2 hours; heat...

Embodiment 2

[0025] The preparation method of sucralose comprises the steps:

[0026] (1) Put 150 grams of sucrose (342.3 grams per mole of sucrose) into N,N-dimethylformamide, then add toluenesulfonic acid and trimethyl orthoacetate, keep stirring at 20°C for 10 hours; add water, Stir at 20°C for 3 hours; add tert-butylamine and stir at 0°C for 3 hours; rectify under reduced pressure at 30mmHg and below 50°C to remove water and part of N,N-dimethylformamide, and obtain a water content of 0.12% Sucrose-6-acetate N, N-dimethylformamide solution, the mol ratio of said sucrose, N, N-dimethylformamide, toluenesulfonic acid, trimethyl orthoacetate, water, t-butylamine is : 1:20:0.03:1.5:5.0:0.5;

[0027] (2) At -15°C, add tetrabutylammonium bromide to N,N-dimethylformamide, then add thionyl chloride, mix to obtain a mixture, and keep it warm for 3 hours; Add 2,4,6-tri-tert-butylphenol to the mixture, then add the solution obtained in step (1), and keep it warm for 3 hours; heat up to 70°C, ke...

Embodiment 3

[0030] The preparation method of sucralose comprises the steps:

[0031] (1) Put 150 grams of sucrose (342.3 grams per mole of sucrose) into N,N-dimethylformamide, then add hydrogen chloride and triethyl orthoacetate, keep stirring at 35°C for 5 hours; Stir at ℃ for 1 hour; add tert-butylamine and stir at 30°C for 1 hour; rectify under reduced pressure at 20mmHg and below 50°C to remove water and part of N,N-dimethylformamide to obtain sucrose with a water content of 0.11% -6-Acetate N, N-dimethylformamide solution, the molar ratio of sucrose, N, N-dimethylformamide, hydrogen chloride, triethyl orthoacetate, water, t-butylamine is: 1:23 :0.015:2.0:8.0:0.2;

[0032](2) At -5°C, add tetrabutylammonium chloride to N,N-dimethylformamide, then add bis(trichloromethyl)carbonate, mix to obtain a mixture, and keep it warm for 2 hours; At 2°C, add tert-butylhydroquinone (TBHQ) to the mixture, then add the solution obtained in step (1), and keep the temperature for 2 hours; heat up to...

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Abstract

The invention discloses a preparation method of sucralose. The preparation method comprises the following steps: (1) adding sucrose into N,N-dimethyl formamide, adding a catalyst, ortho-acetate, water and tert-butylamine and stirring; and conducting vacuum distillation to obtain a sucrose-6-acetate N,N-dimethyl formamide solution; (2) adding a phase transfer catalyst and a chlorination reagent into N,N-dimethyl formamide to obtain a mixture, and reacting; adding an antioxidant and the solution obtained in the step (1) into the mixture, reacting to obtain a sucralose-6-ester reaction solution; and cooling to room temperature, neutralizing, distilling, extracting, concentrating and crystallizing to obtain sucralose-6-acetate; and (3) dissolving sucralose-6-acetate in methanol, regulating the pH value, reacting, neutralizing to remove impurities, decolourizing, concentrating, crystallizing, recrystallizing and drying to obtain sucralose. The invention simplifies the reaction steps, effectively avoids excessive chlorination and polymeric reaction, improves the reaction efficiency, and is beneficial to industrial production.

Description

technical field [0001] The invention relates to a preparation method of sucralose. Background technique [0002] The chemical name of sucralose is 4, 1', 6'--chloro-4, 1', 6'--deoxygalactose, and its chemical structural formula is: [0003] [0004] Sucralose, a new type of high-sweetness non-nutritive sweetener, is 600 times sweeter than sucrose. It has pure sweetness, high safety, good stability, and is not absorbed by the human body. It was synthesized by the British Tate&Lyte Company in 1976 It was successfully put into the market in 1988 and has been approved as a sweetener by many countries including China. Among the various synthesis methods of sucralose that have been reported, both the single-group protection method and the whole-group protection method use sucrose as a raw material. The single-group protection method can synthesize sucralose in three steps, with few steps, simple operation, and low requirements on process equipment, but the yield is low. The ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H5/02C07H1/00
Inventor 万屹东潘春芮新生
Owner CHANGMAO BIOLOGICAL LIANYUNGANG
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