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Method for efficiently synthesizing trichlorosucrose

A high-efficiency technology for sucralose, applied in the field of high-efficiency synthesis of sucralose, can solve the problems of low product purity, low efficiency and low conversion rate, and achieve the effects of high product purity, high selectivity and less organic reagents

Active Publication Date: 2012-02-01
安徽万和制药有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are many methods for synthesizing sucralose with sucralose-6-ethyl ester, but most of them use weak alkaline / methanol system for alcoholysis to produce sucralose, and the efficiency and conversion rate of these methods are not high , the purity of the product is also low

Method used

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  • Method for efficiently synthesizing trichlorosucrose
  • Method for efficiently synthesizing trichlorosucrose
  • Method for efficiently synthesizing trichlorosucrose

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Sucralose was synthesized as follows:

[0016] (1) Alcoholysis: put 25g of sucralose-6-ethyl ester, 50g of methanol, 1.5g of wet Amberlyst-15 into a 250mL reaction bottle, and react at 45°C for 5h; the specific reaction chemical equation is as follows:

[0017]

[0018] (2) Post-treatment: After the reaction is finished, adjust the pH of the reaction solution to 7 and filter, then decolorize with activated carbon and evaporate methanol in a vacuum to obtain a dark red slurry, add anhydrous methanol to heat and dissolve, cool to 5°C, and After standing overnight, 21.2 g of sucralose was obtained after crystallization and purification. After testing, the purity was ≥99%, and the yield was about 84.8%.

Embodiment 2

[0020] Sucralose was synthesized as follows:

[0021] (1) Alcoholysis: Add 25g of sucralose-6-ethyl ester, 50g of methanol, and 1.5g of recovered wet Amberlyst-15 into a 250mL reaction bottle, and react at 45°C for 5h; the specific reaction chemical equation is as follows:

[0022]

[0023] (2) Post-treatment: After the reaction is finished, adjust the pH of the reaction solution to 7 and filter, then decolorize with activated carbon and evaporate methanol in a vacuum to obtain a dark red slurry, add anhydrous methanol to heat and dissolve, cool to 5°C, and After standing overnight, 20.9 g of sucralose was obtained after crystallization and purification. After testing, the purity of the product was ≥99%, and the yield was about 83.6%.

Embodiment 3

[0025] Sucralose was synthesized as follows:

[0026] (1) Alcoholysis: add 25g of sucralose-6-ethyl ester, 50g of methanol, and 1.2g of dry Amberlyst-15 into a 250mL reaction bottle, and react at 45°C for 5h; the specific reaction chemical equation is as follows:

[0027]

[0028] (2) Post-treatment: After the reaction is finished, adjust the pH of the reaction solution to 7 and filter, then decolorize with activated carbon and evaporate methanol in a vacuum to obtain a dark red slurry, add anhydrous methanol to heat and dissolve, cool to 5°C, and After standing overnight, 21.1 g of sucralose was obtained after crystallization and purification. After testing, the purity was ≥99%, and the yield was about 84.4%.

[0029] Practice has proved that, compared with the prior art, the method for synthesizing sucralose of the present invention has simple process and mild reaction conditions; the purity of the products is above 99%, which is higher than that of the prior art above 98...

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Abstract

The invention discloses a method for efficiently synthesizing trichlorosucrose, belonging to the field of organic synthesis. The method comprises the following steps: carrying out alcoholysis on trichlorosucrose-6-ethyl ester in a strong-acid macroporous ion exchange resin / methanol system at 40-70 DEG C, and carrying out after-treatment to obtain the finished trichlorosucrose product. Sucrose-6-ethyl ester, which serves as the raw material, is subjected to alcoholysis reaction to prepare the product in one step. Thus, the method has the advantages of simple technique, mild reaction conditions, high selectivity, high product purity, high yield and easy after-treatment, conforms to requirements for environmental protection, and is very suitable for industrial production.

Description

technical field [0001] The invention relates to a method for synthesizing organic matter, more specifically, an efficient method for synthesizing sucralose. Background technique [0002] Sucralose, namely 4,1',6'-trichloro-4,1',6'-trideoxygalactose, is a new type of sweetener, which is to select the 4,1',6' hydroxyl group of sucrose Its sweetness is 600 times that of sucrose. It does not participate in human metabolism. What is particularly interesting is that it has low calories and can completely replace many products (such as food, candy, beverages, The saccharin and sucralose used in cough medicine tablets) have good chemical stability, are not prone to pyrolysis or hydrolysis reactions, especially have good stability in acidic solutions, and are a promising sweetener. [0003] At present, there are many methods for synthesizing sucralose with sucralose-6-ethyl ester, but most of them use weak alkaline / methanol system for alcoholysis to produce sucralose, and the effici...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H5/02C07H1/00C07H1/06
Inventor 刘海
Owner 安徽万和制药有限公司
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