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Method for preparing sucralose from sucralose-6-acetate

A technology for sucralose and chlorinating reagents, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of large material loss, high production cost, and high energy consumption for solvent recovery, reducing The effect of energy consumption, reduction of solvent consumption and improvement of production technology level

Active Publication Date: 2012-12-05
HUBEI YITAI PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

From the above preparation of sucralose, it can be seen that from the reaction solution of sucralose-6-ester to the finished product of sucralose, there are many processing procedures, large solvent consumption, high energy consumption for solvent recovery, large material loss and high production cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A method for preparing sucralose from sucralose-6-ester, which includes the following steps: first prepare Vilsmeier reagent with a chlorinating reagent, add the DMF solution of sucrose-6-ester dropwise at 5-10°C, and increase the temperature To 108-109 ℃, keep for 2.5 hours, concentrate under reduced pressure to distill out fat-soluble solvent (toluene, dichloroethane or trichloroethane). The material liquid is cooled down to obtain a sucralose-6-ester reaction liquid. Take the reaction solution of sucralose-6-ester as raw material, add 30% lye dropwise at 5-35℃, adjust PH=12-14, keep for 1-3 hours, hydrolyze to obtain the reaction solution of sucralose, use ethyl acetate The mixture of ester:n-butanol=4-20:1 is extracted three times, concentrated in vacuo to remove the solvent, and water is added to cool and crystallize to obtain crude sucralose. The crude sucralose is refined by adding water to obtain sucralose.

Embodiment 2

[0017] A method for preparing sucralose from sucralose-6-ester, which includes the following steps: first prepare a Vilsmeier reagent with a chlorinating reagent, add the DMF solution of sucrose-6-ester dropwise at 5°C, and raise the temperature to 108 Keep it at ℃ for 2.5 hours, concentrate under reduced pressure and distill out fat-soluble solvent (toluene, dichloroethane or trichloroethane). The material liquid is cooled down to obtain a sucralose-6-ester reaction liquid. Take sucralose-6-ester reaction solution as raw material, add lye dropwise at 5℃, adjust PH=12, keep for 1 hour, hydrolyze to obtain sucralose reaction solution, use ethyl acetate:n-butanol=3: Extract the mixed solvent of 1 for 3 times, concentrate in vacuo to remove the solvent, add water to cool and crystallize to obtain crude sucralose. The crude product is refined by adding water to obtain sucralose.

Embodiment 3

[0019] A method for preparing sucralose from sucralose-6-ester, which includes the following steps: first prepare a Vilsmeier reagent with a chlorinating reagent, add the DMF solution of sucrose-6-ester dropwise at 10°C, and heat to 109 Keep it at ℃ for 2.5 hours, concentrate under reduced pressure and distill out fat-soluble solvent (toluene, dichloroethane or trichloroethane). The material liquid is cooled down to obtain a sucralose-6-ester reaction liquid. Take the reaction solution of sucralose-6-ester as the raw material, add dropwise lye with a concentration of 30% at 35℃, adjust the PH=14, keep it for 3 hours, hydrolyze to obtain the reaction solution of sucralose, use ethyl acetate: normal Extraction with butanol=20:1 mixed solvent for 3 times, vacuum concentration to remove the solvent, add water to cool and crystallize to obtain crude sucralose. The crude product is refined by adding water to obtain sucralose.

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PUM

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Abstract

The invention discloses a method for preparing sucralose from sucralose-6-acetate. The method comprises the following steps of: adding alkali into reaction liquid of sucralose-6-acetate serving as a raw material at the temperature of between 5 and 35DEG C to regulating the pH to be 12-14, keeping the temperature for 1 to 3 hours, and performing hydrolysis to obtain reaction liquid of sucralose; extracting for 3 to 5 times by using a mixed solvent of ethyl acetate and n-butyl alcohol in a ratio of (3-20):1; concentrating in vacuum to remove the solvent; and adding water and cooling for crystallization to obtain a crude product of sucralose; and adding water and refining the crude product to obtain the sucralose. The method has the advantages that: multiple steps from the reaction liquid ofthe sucralose-6-acetate to the crude product of the sucralose-6-acetate to the pure product of the sucralose are eliminated, energy consumption is effectively reduced, the consumption of the solvent is reduced, and the technological level is improved.

Description

Technical field [0001] The invention relates to the technical field of preparation of sucralose, in particular to a method for preparing sucralose from sucralose-6-ester with a simple process. Background technique [0002] Sucralose is a high-sweetness, non-calorie sweetener. In the previous synthetic preparation literature of sucralose and the current domestic large-scale production process, sucrose is used as a raw material, first converted into sucrose-6-ester, and then sucrose-6-ester is chlorinated to obtain sucralose-6-ester , The sucralose is obtained by alcoholysis. After the chlorination reaction is completed, the sucralose intermediate-sucralose-6-ester crude product must be obtained through the following process: that is, add alkali to neutralize to pH=7, centrifuge to remove salt, and use ethyl acetate for the obtained material liquid The ester is extracted 5-6 times, concentrated under reduced pressure to remove ethyl acetate, and the residue is crystallized with w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H5/02C07H1/00
Inventor 王正友
Owner HUBEI YITAI PHARMA