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Preparation method of trichlorosucrose-6-acetate

A technology of sucralose and acetate, which is applied to the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of bad smell, high price, and high cost, and achieve fewer reaction steps, low cost, and The effect of reducing side effects

Inactive Publication Date: 2013-03-20
CHANGZHOU NIUTANG CHEM PLANT CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As far as the applicant knows, regarding the sucralose intermediate: the preparation method of sucralose-6-acetate, there are the following defects in the prior art: US Pat. Reaction with phosgene in medium, then obtain sucralose-6-acetate through processing, this method yield is lower
In the British patent GB2222827A, pyridine is used as an organic base, thionyl chloride is used as a chlorinating agent, and trichloroethane is used as a solvent for the reaction. After treatment, sucralose-6-acetate is obtained. The disadvantage of this method is that a large amount of Expensive, foul-smelling pyridine at very high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] This embodiment is the method of obtaining sucralose-6-acetate without using ethyl chloride as the reaction solvent:

[0016] Drop 150 grams of thionyl chloride into 650 ml of DMF solution containing 40 grams of sucrose-6-acetate, and the temperature during the dropping process should not exceed 5°C; The temperature was raised to 80° C. for 1 hour, the temperature was raised to 100° C. for 1 hour, and finally the temperature was raised to 110-113° C. for 2 hours to obtain a reaction solution. Cool the reaction solution to 0°C, add 20% liquid caustic soda dropwise to pH 9, and then neutralize it with hydrochloric acid; evaporate the solvent to a sticky substance, add water to dissolve, and filter. It was extracted with ethyl acetate, decolorized and concentrated to obtain a viscous substance, which was dissolved in water, cooled, crystallized and dried to obtain 26.5 g of sucralose-6-acetate with a yield of 57.8%.

Embodiment 2

[0018] Pour 150 grams of thionyl chloride into 600 ml of 1,1,2-trichloroethane, then add 65 ml of DMF solution containing 40 grams of sucrose-6-acetate dropwise to the above solution, the temperature during the dropwise addition No more than 5°C; after the dropwise addition, slowly raise the temperature to 60°C for half an hour, raise the temperature to 80°C for 1 hour, raise the temperature to 100°C for 1 hour, and finally raise the temperature to 110-113°C for 2 hours to obtain a reaction solution. Cool the reaction solution to 0°C, add 20% liquid caustic soda dropwise to pH 9, and then neutralize it with hydrochloric acid; evaporate the solvent to a sticky substance, add water to dissolve, and filter. Extract with ethyl acetate, decolorize, concentrate the viscous matter, add water to dissolve, cool, crystallize and dry to obtain 32.5 g of sucralose-6-acetate, yield 70.9%.

Embodiment 3

[0020] Add 135 grams of bis-trichloroformic acid carbonate into 600 ml of 1,1,2,2-tetrachloroethane liquid, then add 65 ml of DMF solution containing 40 grams of sucrose-6-acetate dropwise to the above solution, drop The temperature during the addition process does not exceed 5°C; after the dropwise addition, slowly raise the temperature to 60°C for half an hour, heat up to 80°C for 1 hour, heat up to 100°C for 1 hour, and finally raise the temperature to 110-113°C for 2 hours Obtain the reaction solution. Cool the reaction solution to 0°C, add 20% liquid caustic soda dropwise to pH 9, and then neutralize it with hydrochloric acid; evaporate the solvent to a sticky substance, add water to dissolve, and filter. Extract with ethyl acetate, decolorize and concentrate the viscous matter, add water to dissolve, cool, crystallize and dry to obtain 30.0 g of sucralose-6-acetate with a yield of 65.4%.

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Abstract

The invention relates to a preparation method of an intermediate of the food sweetening agent trichlorosucrose, belonging to the technical field of fine chemicals. The theory of the invention is as follows: chloroethane is used as reaction solvent, thus replacing dimethyl formamide (DMF) which is generally used as solvent; and DMF is used as catalyst, thereby greatly reducing the dosage of DMF and saving the cost; and the generated hydrogen chloride and sulfur dioxide can fast leave the reaction system, thereby reducing side reactions. The preparation method has the following beneficial effects; the method has low cost and less reaction steps, the yield is obviously improved by about 20% compared with the method using DMF as solvent, and the preparation method has obvious advantages.

Description

technical field [0001] The invention relates to a preparation method of an intermediate of food sweetener sucralose, belonging to the technical field of fine chemicals. Background technique [0002] Sucralose is a healthy functional sweetener. It is the only strong sweetener made from sucrose through chlorination. It has the advantages of health, greenness, functionality and safety. Its chemical name is 4,1',6'-trichloro-4,1',6'-trideoxygalactose, also known as sucralose, it is a white powder product, easily soluble in water, ethanol and Methanol has a water solubility of over 25% at room temperature. Sucralose is not prone to foaming when dissolved in water and is easy to dilute. It also has good solubility in alcohol and is suitable for use in the production of alcoholic beverages. The sweetness of sucralose is 600 times that of sucrose, and the sweetness is pure, and it has the characteristics of high safety and good stability. Sucralose does not participate in metaboli...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H13/06C07H1/00
Inventor 蔡亚王立成高正兵王立平
Owner CHANGZHOU NIUTANG CHEM PLANT CO LTD
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