Preparation method of sucralose

A technology for sucralose and sucralose, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of low yield of sucralose, etc. short time effect

Active Publication Date: 2010-08-25
南通宏信化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of the above-mentioned single-group protection method is: the acetylation reagent selected in the acylation reaction

Method used

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  • Preparation method of sucralose

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

Example 1:

(1) Acylation reaction

Add 50g sucrose (0.146mol) and 200ml N,N dimethylformamide (DMF) into a 500ml four-necked flask (equipped with mechanical stirring, thermometer, condenser, drying tube), and reduce the temperature of the reaction system to -20 At a temperature of ℃, 6.15g (0.146mol) of ketene gas was introduced, which was completed within 1 hour. After the reaction, the solvent N,N dimethylformamide (DMF) was distilled off under reduced pressure, 100ml methanol was added to the residue and heated to dissolve, stirred, the temperature dropped to room temperature and then left until white crystals appeared, filtered and placed in vacuum In a drying oven to constant weight, 46.8 g of white solid was obtained. The melting point is 90-92°C, the purity of sucrose-6-acetate analyzed by high performance liquid chromatography is 97.2%, and the yield is 79%.

(2) Chlorination reaction

Add 46.8g of sucrose-6-acetate obtained in the previous step and 200ml of N,N dimeth...

Example Embodiment

Example 2:

(1) Acylation reaction

In a 5L reactor (equipped with mechanical stirring, thermometer, condenser, drying tube), add 500g sucrose (1.46mol) and 2L N,N dimethylformamide (DMF), and reduce the temperature of the reaction system to -30 At a temperature of ℃, 61.5g (1.46mol) of ketene gas was introduced, which was completed within 1 hour. After the reaction, the solvent N,N dimethylformamide (DMF) was distilled off under reduced pressure, and 1L of methanol was added to the residue and heated to dissolve, stirred, the temperature dropped to room temperature and then left until white crystals appeared, filtered, and placed in vacuum In a dry box to constant weight, 477.8 g of white solid was obtained. The melting point is 90.8-92.2°C, and the purity of sucrose-6-acetate analyzed by high performance liquid chromatography is 97.7%.

(2) Chlorination reaction

Add 477.8g of sucrose-6-acetate obtained in the previous step and 2L of N,N dimethylformamide (DMF) solvent into a...

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Abstract

The invention discloses a method for preparing sucralose by using a new acetylation reagent, which comprises the following steps: (1) acylation reaction: reacting sucrose with acetylation reagent to produce sucrose-6-acetate; (2) chlorination reaction: carrying out chlorination reaction on the sucrose-6-acetate obtained in the step (1) to obtain sucralose-6-acetate; (3) and deacetylation reaction: carrying out deacetylation reaction on the sucralose-6-acetate obtained in the step (2) to obtain sucralose. The ketene gas used in the acylation reaction is used as the acetylation reagent. The method can effectively increase the sucralose yield, and has the advantages of short reaction time, easy control of reaction temperature, and easy realization of industrial production.

Description

technical field The invention relates to a method for synthesizing sweetener sucralose, and further relates to a method for preparing sucralose by using sucrose and organic reagents as raw materials and adopting a single-group protection method. Background technique Sucralose, chemical name 4,1',6'-trichloro-4,1'6'trideoxygalactose, its sweetness is 600 times that of sucrose, widely used in beverages, chewing gum, bread, jelly and other foods In addition, its application in the field of medicine is also expanding. Using sucrose and organic reagents as raw materials, the method for preparing sucralose by the single-group protection method includes the following three process steps: (1) acylation reaction, first dissolving sucrose in an organic solvent, then adding acetylating reagents for reaction, and reacting After finishing, remove solvent and filter and dry to obtain sucrose-6-acetate; (two) chlorination reaction, the sucrose-6-acetate that first step reaction is obtaine...

Claims

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Application Information

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IPC IPC(8): C07H5/02C07H1/00
Inventor 陈小萍陈颖刘纪才
Owner 南通宏信化工有限公司
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