Purification method of saccharose-6-acetate

A purification method, acetate technology, applied in the field of purification of sucrose-6-acetate, can solve the problem of large solvent consumption

Inactive Publication Date: 2019-04-09
ANHUI JINGHE IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the defects of low purity and large solvent consumption in the purification of sucrose-6-acetate in the prior art, and provide a kind of convenient operation, high yield, low separation cost, and the purity can reach 97%. The purification method of above sucrose-6-acetate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Distill 60ml of the DMF solution of sucrose-6-acetate at 65°C and a pressure of -0.09Mpa under reduced pressure. When the pressure is reduced to 25% of the remaining solution, the temperature is raised to 70°C, and most of the DMF is distilled out, leaving about 25% of the volume. Add trimethylpentane under normal pressure and stir at 50°C for half an hour. The volume of trimethylpentane and sucrose-6-acetate is 3:1, and there is a large amount of sucrose-6-acetate The ester crystals were precipitated, filtered with a Buchner funnel, and dried in a drying oven to obtain 6.73 g of crystals. Loss of sucrose-6-acetate was 0.13 g. The obtained sucrose-6-acetate was analyzed by liquid chromatography, and the purity of sucrose-6-acetate was 95%.

Embodiment 2

[0018] Distill the DMF solution of sucrose-6-acetate under the condition of vacuum distillation to remove most of the DMF, leaving 25% of the volume remaining, raise the temperature to 60°C, add trimethylpentane, trimethylpentane and sucrose-6 - The volume of the acetate is 3:1, a large amount of crystals precipitated, filtered and dried in a drying oven to obtain 6.68g of crystals. 0.11 g of sucrose-6-acetate was lost. The obtained sucrose-6-acetate was analyzed by liquid chromatography, and the purity of sucrose-6-acetate was 96%.

Embodiment 3

[0020] Distill the DMF solution of sucrose-6-acetate under the condition of vacuum distillation to remove most of the DMF, and the remaining 25% of the volume, raise the temperature to 70°C, add trimethylpentane, trimethylpentane and sucrose-6 - The volume of the acetate is 3:1, a large amount of crystals precipitated, filtered and dried in a drying oven to obtain 6.65 g of crystals. Loss of sucrose-6-acetate was 0.14 g. The obtained sucrose-6-acetate was analyzed by liquid chromatography, and the purity of sucrose-6-acetate was 96%. It is concluded that the higher the temperature is, the higher the purity of the sucrose-6-acetate obtained by adding trimethylpentane is, and the temperature has less influence on the solubility of sucrose-6-acetate in trimethylpentane.

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Abstract

The invention relates to a purification method of saccharose-6-acetate. The purification method comprises the following steps: (1) distilling a saccharose-6-acetate solution dissolved in an organic solvent DMF at a reduced pressure at 45-65 DEG C, raising the temperature to 50-70 DEG C when the pressure is reduced till the volume of the solution is 25% of the original volume, then adding one of ora combination of more of the following solvents: trimethylpentane, butyryl chloride, trichloro ethylene and chloroform, wherein the volume ratio of the solvents and saccharose-6-acetate is 1.5: 1 to8: 1, and reducing the temperature to 25-40 DEG C; and after analyzing saccharose-6-acetate crystals, filtering the crystals and drying the same to obtain purified saccharose-6-acetate. The solvent ispreferably trimethylpentane. The purification method has the advantages that the amount of needed trimethylpentane is small, the reaction conditions are relatively low, and the purity of the obtainedsaccharose-6-acetate reaches 95-97% or above.

Description

technical field [0001] The invention belongs to a method for purifying a sucralose intermediate, in particular to a method for purifying sucrose-6-acetate. Background technique [0002] Sucralose (TGS), a new type of sweetener jointly developed by Tate & Lyie and the University of London and applied for a patent in 1976. It is the only functional sweetener that uses sucrose as raw material. The original brand name is Splenda, and its sweetness can reach 600 times that of sucrose. Sucralose is a non-hygroscopic white crystalline powder with good stability. This sweetener has the characteristics of no energy, high sweetness, pure sweetness, and high safety. It is one of the best functional sweeteners at present. [0003] In the synthesis of sucralose reported in the literature, the separation and purification of sucrose-6-acetate are relatively rare, and generally directly participate in subsequent reactions. However, the disadvantages of the direct reaction are also obviou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H13/06C07H1/06
CPCC07H1/06C07H13/06
Inventor 赵程成姜维强易建康
Owner ANHUI JINGHE IND
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