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Method of preparing sucralose

A technology for sucralose and sucralose, which is applied in the field of preparation of sucralose, can solve the problems of high production cost, cumbersome process, unsatisfactory chemical yield of sucralose-6-ester and product purity, etc., and achieves conversion rate and purity. High, mild reaction conditions, the effect of reducing production costs

Inactive Publication Date: 2008-09-24
CHIFENG BROAD BIOLOGICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] There are many reaction steps in the whole group protection method, and the process is relatively cumbersome
However, the chemical yield and product purity of the existing single-group protection method for synthesizing sucrose-6-ester are not ideal, and the catalyst dibutyltin oxide of the dibutyltin oxide method cannot be recycled, and the production cost is high

Method used

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  • Method of preparing sucralose
  • Method of preparing sucralose
  • Method of preparing sucralose

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Preparation of sucrose-6-ethyl ester:

[0041] Add 200g (0.585mol) sucrose, 0.5g (6.13mmol) P4SnBu to the reaction flask 2 Cl, 700ml DMF and 200ml cyclohexane, heated to reflux, kept reflux for 5h after the solution was clarified, drained the water in the water separator, and added an appropriate amount of cyclohexane to keep the reaction temperature at 92°C. The solution was cooled to 5°C, and 65 g (0.637 mol) of acetic anhydride was added dropwise within 10 minutes, and the maximum temperature did not exceed 10°C. Stirring was continued for 1 h after the dropwise addition. The reactant was poured into 50ml of water and extracted with cyclohexane. After phase separation, the DMF layer was poured into 50ml of water and 250ml of DMF, continuously extracted with cyclohexane for 3 times, and the 4 times of cyclohexane layers were combined to recover the catalyst. The DMF layer was evaporated to remove the solvent under reduced pressure to obtain almost quantitative yell...

Embodiment 2

[0047] Preparation of sucrose-6-ethyl ester:

[0048] Add 200g (0.585mol) sucrose, 0.26g (3.07mmol) P4SnBu to the reaction flask 2Cl, 700ml DMF and 200ml cyclohexane, heated to reflux, kept reflux for 5h after the solution was clarified, drained the water in the water separator, and added an appropriate amount of cyclohexane to keep the reaction temperature at 92°C. The solution was cooled to 5°C, and 89 g (0.872 mol) of acetic anhydride was added dropwise within 10 minutes, and the maximum temperature did not exceed 10°C. Continue to stir for 0.5h after the dropwise addition. The reactant was poured into 80ml of water and extracted with cyclohexane. After phase separation, the DMF layer was poured into 80ml of water and 250ml of DMF, continuously extracted with cyclohexane for 3 times, and the 4 times of cyclohexane layers were combined to recover the catalyst. The DMF layer was evaporated to remove the solvent under reduced pressure to obtain 190 g of yellow syrup sucrose...

Embodiment 3

[0054] Preparation of sucrose-6-ethyl ester:

[0055] Add 200g (0.585mol) sucrose, 1g (12.3mmol) P4SnBu to the reaction flask 2 Cl, 700ml DMF and 200ml cyclohexane, heated to reflux, kept reflux for 5h after the solution was clarified, drained the water in the water separator, and added an appropriate amount of cyclohexane to keep the reaction temperature at 92°C. The solution was cooled to 5°C, and 70 g (0.686 mol) of acetic anhydride was added dropwise within 10 minutes, with the maximum temperature not exceeding 10°C. Continue to stir for 2h after the dropwise addition. The reactant was poured into 80ml of water and extracted with cyclohexane. After phase separation, the DMF layer was poured into 80ml of water and 250ml of DMF, continuously extracted with cyclohexane for 3 times, and the 4 times of cyclohexane layers were combined to recover the catalyst. The DMF layer was evaporated to remove the solvent under reduced pressure to obtain 213 g of sucrose-6-ethyl ester in...

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Abstract

The invention discloses a making method of trichlorine saccharide, which comprises the following steps: reacting saccharose and acylating agent under organic tin catalyst loaded by polymer to produce high-chemical purity saccharose-6-ester; chlorinating; hydrolyzing; obtaining the product.

Description

technical field [0001] The invention relates to a preparation method of sucralose. Background technique [0002] Sucralose is a new type of high-sweet non-nutritive sweetener, the chemical name is 4,1',6'-trichloro-4,1',6'-trideoxygalactosucrose, English Name: 4,1′,6′-trichlorogalactosucrose 1,6-dichloro-1,6-dideoxy-β-D-fructofuran-nosyl-4-chloro-4-deoxy-α-D-galactopyranoside. [0003] The chemical structural formula is as (I): [0004] [0005] The sweetness of sucralose is about 600 times that of sucrose. It does not participate in metabolism in the human body, is not absorbed by the human body, and has 0 calories. It is an ideal sweet substitute for diabetics. In addition, sucralose cannot be utilized by dental caries bacteria and will not cause dental caries. It has been approved as a food sweetener by more than 20 countries. [0006] Sucralose was synthesized by British Tate & Lyle Company in 1975. The chemical synthesis methods mainly include single group prote...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H5/02
Inventor 李金亮
Owner CHIFENG BROAD BIOLOGICAL TECH CO LTD
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