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Method of preparing sucralose

A technology of sucralose and sucrose, which is applied in the direction of chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve the problems of difficult preparation, residue pollution, difficult recovery, etc., and achieve high yield and low production cost Effect

Inactive Publication Date: 2008-02-13
JIANGSU JUBANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The purpose of the present invention is to address the shortcomings of the existing sucralose single-protection route production process, such as the difficulty in preparing the intermediate sucrose-6-acetate in the lipidation protection step, and the presence of the catalyst itself in the chlorination step. Provide a new method for the preparation of sucralose by producing difficult-to-remove by-products or catalysts that are expensive, use a large amount, are difficult to recycle, and residues pollute products.

Method used

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  • Method of preparing sucralose

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Effect test

Embodiment 1

[0025] Sucrose 3.42g (0.01mol), DMF 20ml, heated up at 90°C to dissolve, cooled to room temperature, added p-toluenesulfonic acid 0.05g and vinyl acetate 0.96 / g (0.011mol), stirred at room temperature for 12 hours, followed by TLC until the sugar basically disappeared . After removing excess vinyl acetate and by-product acetaldehyde under reduced pressure, adjust the pH to 9-9.5 with tert-butylamine: heat up at 40°C for two hours, evaporate DMF under reduced pressure to obtain sucrose-6-acetate syrup 5.1 g, the measured content of sucrose-6-acetate was 66.1%, and the yield was 87.8%.

Embodiment 2

[0027] Sucrose 34.2g (0.1mol) DMF 200ml, warm up to complete dissolution, cool, add p-toluenesulfonic acid 0.5g and vinyl acetate 9.7g (0.112mol), stir at room temperature for 12 hours overnight. TLC showed that there was almost no sucrose, vinyl acetate and by-product acetaldehyde were removed under reduced pressure, the pH was adjusted to 9-9.5 with tert-butylamine, the temperature was raised to 40°C and kept for 2 hours, DMF was evaporated under reduced pressure to obtain 52.8g of syrup, and the measured sucrose- The content of 6-acetate is 64.5%, and the yield is 88.7%.

Embodiment 3

[0029] Sucrose 171g (0.5mol) DMF 1000ml, in a 2000ml four-neck bottle, heated to complete dissolution, cooled to room temperature, added 1.0g benzenesulfonic acid and 48.60g (0.565mol) vinyl acetate, stirred overnight at room temperature, almost no sucrose as measured by TLC, Remove excess raw materials and by-products under reduced pressure, adjust the pH to 9-9.5 with tert-butylamine, raise the temperature at 40°C and keep for 2 hours, evaporate DMF under reduced pressure to obtain 267.8 g of syrup, and the content of sucrose-6-acetate was measured to be 62.7%. Yield 87.4%.

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Abstract

The invention relates to a preparation method of food sweetener-sucralose, comprising the steps of preparing sucrose-6-ester from sucrose, and preparing 1',4,6'-trichlorosucrose by chlorination of sucrose-6-ester -1',4,6'-trideoxygalactosucrose-6-ester step and deesterification step to prepare sucralose; it is characterized in that the preparation of sucrose-6-ester is that sucrose is in DMF solvent, in acidic React with enol ester in the presence of catalyst to obtain sucrose-6-ester. The acidic catalyst is any one of benzenesulfonic acid, p-toluenesulfonic acid, and dibutyltin oxide. Enol esters include vinyl acetate and isopropenyl benzoate. The chlorination reaction is carried out under the conditions of using organic tertiary amine as a catalyst and changing the polarity of the solvent. The yield of each reaction step of the invention is high, the content of the obtained finished product is as high as 99%, the production cost is low, and it is suitable for industrialized production.

Description

technical field [0001] The invention relates to a preparation method of food sweetener-sucralose. Background technique [0002] The chemical name of sucralose is 1',4,6'-trichloro-1',4,6'-trideoxygalactosucrose, which is a new type of strong sweetener, which is characterized by high sweetness and is sucrose 600 times that of sucrose; the sweetness is pure, the taste is basically the same as that of sucrose; the performance is stable, and it is not easy to be damaged by harsh environments such as acid, alkali, and high temperature; it has a wide range of applications and can be used in almost all foods, and it is safe to use in food; Non-rodent, suitable for diabetics and dental patients. The chemical structural formula of sucralose is: [0003] [0004] The preparation technology of existing sucralose is basically carried out according to the following steps: [0005] Sucrose → esterification protection → selective chlorination → deprotection group → sucralose, wherein...

Claims

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Application Information

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IPC IPC(8): C07H5/02
Inventor 蒋志平杨浩平魏松林国胜陆丽君于建福
Owner JIANGSU JUBANG PHARMA
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