Low-temperature and efficient preparation method of sucrose-6-acetate

A technology of acetate and sucrose, which is applied in the field of preparation of intermediate sucrose-6-acetate, can solve the problem of low conversion rate of sucrose-6-acetate, reduce the difficulty of solvent treatment, and facilitate batch production Production, production stable effect

Inactive Publication Date: 2017-05-10
TECHNO (FUJIAN) FOOD INGREDIENTS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to overcome the deficiencies in the prior art, to provide a low-temperature and high-efficiency preparation method of sucrose-6-acetate with low tem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A low-temperature and high-efficiency preparation method of sucrose-6-acetate in this embodiment, the steps are as follows:

[0016] (1) Add 34.2g (0.1mol) sucrose and 342.1g (4.62mol) DMF into a 1000ml three-necked flask, and dissolve the sucrose completely at 80°C; then cool down to 60°C, add 55.0g (0.0917mol) DSDA and Mix 150.2g (1.78mol) of cyclohexane to form a mixed catalyst solution, stir at 60°C and a vacuum of -0.05Mpa, use a water separation and reflux device to carry out a low-temperature vacuum reflux and water separation reaction for 6 hours, maintain cyclohexane reflux, and Remove the generated water until the mass concentration of water in the system is 0.101%, and the color is light yellow;

[0017] (2) After the water separation, 12.0g (0.1017mol) acetic anhydride was added at -5°C, and then kept at 0°C for 4 hours, and then 25.3g (0.141mol) of water was added to stop the reaction to obtain sucrose-6- Acetate; 150.1 g (1.78 mol) cyclohexane was added t...

Embodiment 2

[0020] The low-temperature and high-efficiency preparation method of sucrose-6-acetate in this example differs from Example 1 in that the low-temperature vacuum reflux temperature in step (1) is 68°C, and the vacuum degree is -0.04Mpa. The mass concentration of water is 0.124%, and the color is yellow.

[0021] As determined by HPLC, the molar residual sucrose of the sucrose-6-acetate sample in this example was 2.12%, and the molar yield of sucrose-6-acetate was 86.3%.

Embodiment 3

[0023] A low-temperature and high-efficiency preparation method of sucrose-6-acetate in this embodiment differs from Example 1 in that: the catalyst mixed solution in step (1) uses the DSDA containing cyclohexane recycled in Example 1, The mass concentration of water in the system is 0.104%, and the color is yellow.

[0024] As determined by HPLC, the molar residual sucrose of the sucrose-6-acetate sample in this example was 2.12%, and the molar yield of sucrose-6-acetate was 87.32%.

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Abstract

The invention discloses a low-temperature and efficient preparation method of sucrose-6-acetate. The method comprises the steps of dissolving sucrose into an organic solvent, mixing with an organic tin acylation accelerator containing a cosolvent, removing generated water in vacuum and low-temperature conditions; and adding carboxylic acid anhydride at 0 DEG C for thermal reaction and terminating reaction through adding water to obtain the sucrose-6-acetate. The preparation process of the sucrose-6-acetate is low in temperature, thorough in dehydration and stable in production; the obtained product is high in purity, especially the sucrose residue content is low; the difficulty of subsequently removing 6'-tetradeoxygalactosucrose is reduced; and the yield of the sucrose-6-acetate is high. In addition, the organic tin acylation accelerator can be utilized in cycle without removing the cosolvent, the difficulty of solvent treatment in the preparation process is reduced, and massive production is facilitated.

Description

technical field [0001] The invention relates to the technical field of sucralose production, in particular to a preparation method of sucralose intermediate sucrose-6-acetate. Background technique [0002] Sucralose (TGS for short) is a synthetic high-intensity sweetener that is very suitable for use in food and beverages. Sucrose-6-acetate is an important intermediate in the synthesis of sucralose. At present, its preparation methods mainly include orthoester method and organotin method. However, the biggest disadvantage of the orthoester method is that the conversion rate of sucrose-6-acetate is low and the residual sucrose is high, resulting in more tetrachloral sucrose as an impurity after chlorination, which increases the difficulty of purification of subsequent products; while sucrose in the organotin method The dehydration reaction with organotin has a key influence on the yield of sucrose-6-acetate, but the existing technology generally has technical defects such as...

Claims

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Application Information

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IPC IPC(8): C07H13/06C07H1/00
CPCC07H13/06C07H1/00
Inventor 郭振明陈建峰施俊戴燕斌
Owner TECHNO (FUJIAN) FOOD INGREDIENTS CO LTD
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