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Technique for synthesizing and purifying sucrose trichloride

A synthesis process, the technology of sucralose, applied in the field of synthesis and purification process of sucralose, can solve the problems of high production cost, cumbersome process, unfavorable application, etc., achieve high conversion rate and purity, mild reaction conditions, reduce production cost effect

Inactive Publication Date: 2008-08-20
HUBEI YITAI PHARMA
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Problems solved by technology

[0014] Among these synthetic methods, the whole group protection method has many reaction steps, the process is relatively cumbersome, and the production cost is high; the chemical yield of the sucrose-6-ester synthesized by the single group protection method is low and the product aqueous phase purification is difficult and complicated, and The purity is not very ideal; the catalyst dibutyltin oxide of the dibutyltin oxide method cannot be recycled, the production cost is high, and the product contains tin-based impurities, which is not conducive to application

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  • Technique for synthesizing and purifying sucrose trichloride

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Embodiment Construction

[0040] Below in conjunction with specific embodiment, further illustrate the present invention. It should be understood that these examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention.

[0041] Synthesis of Sucrose-6-Acetate

[0042] Add 100g sucrose, 350ml N, N-dimethylformamide, 100ml cyclohexane, 2g catalyst (sodium acetate: DMAP=0.5: 1.5) in a 1000ml four-neck flask, heat to reflux, and dehydrate for 3 hours under stirring , then cooled to 25°C, added dropwise 40g of acetic anhydride, and then incubated for 5 hours, filtered to recover the catalyst, and the mother liquor was decompressed to recover DMF to obtain 108g of syrup. Ester 90.2%.

[0043] Synthesis of Sucralose-6-Acetate

[0044] Take the above 108g syrup and dissolve it with 500ml N,N-dimethylformamide for later use, add 500ml N,N-dimethylformamide into a 2000ml four-necked bottle, cool to -10°C, add 300ml thionyl chloride dropwise, contro...

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Abstract

The invention discloses a technique of the synthesis and the purification of sucralose; in the synthetic technique, with the existence of organic composite alkali metal salt catalyst, sucrose reacts with an acylating agent in an amides solvent to generate sucrose-6-acetic ester with high chemical yield and purity; then the sucrose-6-acetic ester is subject to chlorination, filtration, extraction and decolourization to prepare an intermediate of the sucralose-6-acetic ester; finally, the intermediate of sucralose-6-acetic ester is subject to acyl removal and decolourization in an anhydrous solvent system to generate the sucralose; in the purification technique, a component solvent is adopted to carry out purification to the crude product of the sucralose so as to obtain the sucralose. The technique of the synthesis and purification of sucralose has the advantages of simple technique, high chemical yield and purity of products and low production cost, and is extremely suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a synthesis and purification process of sucralose. Background technique [0002] Sucralose, chemical name 4,1',6'-trichloro-4,1',6'-trideoxygalactosucrose, [0003] The English name is: 4,1',6'-trichlorogalactosucrose [0004] Its structural formula is: [0005] [0006] Sucralose is a new type of high-sweetness non-nutritive sweetener. Its sweetness is 600 times that of sucrose. It does not participate in metabolism in the human body, is not absorbed by the human body, is not used by dental caries bacteria, and does not cause dental caries. An ideal sweet substitute for diabetics, it has been approved as a food sweetener by more than 20 countries. [0007] The preparation of sucralose was first successfully prepared by chemical synthesis in 1975 by British Tate & Lyle Company. The chemical synthesis methods mainly include single group protection method and whol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H5/02
CPCC07H5/02C07H1/06Y02P20/582
Inventor 陈新民彭建新
Owner HUBEI YITAI PHARMA
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