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A kind of purification method of sucrose-6-acetate

A purification method and technology of acetate, which is applied in the field of purification of sucralose-6-acetate, can solve the problems of low purity of sucralose-6-acetate, prolonged production cycle, complicated process, etc., to improve the purity and product quality, reduce purification costs, and reduce production costs

Active Publication Date: 2016-04-20
HUBEI HONGYUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, there are two problems in directly chlorinating sucralose as raw material with the sucralose-6-acetate synthesized by the aforementioned two methods: one: the prepared sucralose-6-acetate has low purity, and the sucralose-6-acetate obtained by The purity of the sucralose finally prepared by the above two methods is about 50% (trimethyl orthoacetate method) and about 60% (dibutyltin oxide method), respectively. In order to prepare qualified sucralose products, Need to go through multiple recrystallizations, which makes the production cycle longer and the product yield lower
[0007] When the inventor used the above method to purify sucrose-6-acetate, he found that this method is suitable for purifying a mixture of various sucrose fatty acid esters, and cannot be separated into monomer sucrose fatty acid esters, and there is also the problem of low product recovery , so it is not suitable for the purification process of sucrose-6-acetate; at the same time, the method process is more complicated and the purification cost is higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Inject 2 / 3 of the volume of petroleum ether into the 2m-high chromatographic column, and put in coarse-pore silica gel (200-300 mesh) from the feeding port to about 3 / 5 of the height of the chromatographic column, stir while pouring, and then let it stand About 3h. Open the outlet valve to lower the liquid level of petroleum ether in the chromatography column to 5-10 cm above the top surface of the silica gel.

[0026] Add about 1.5 times (w / v, g / mL) of petroleum ether to the crude product of sucrose-6-acetate prepared by the trimethyl orthoacetate method, stir vigorously to form an emulsion, and then mix with 2 times (w / w ) coarse-pore silica gel (200-300 mesh) and mix well, put it into the above-mentioned silica gel column, and fill it to about 4 / 5 of the height of the chromatography column.

[0027] Rinse the column with a mixed solution of petroleum ether and ethyl acetate (v / v=90:10), discard the fraction without sucrose-6-acetate, and start collecting when sucros...

Embodiment 2

[0029] Inject 2 / 3 of the volume of petroleum ether into the 3m-high chromatographic column, and put in coarse-pore silica gel (200-400 mesh) from the feeding port to about 3 / 5 of the height of the chromatographic column, stir while pouring, and then let it stand About 3h. Open the outlet valve to lower the liquid level of petroleum ether in the chromatography column to 5-10 cm above the top surface of the silica gel.

[0030] Add about 2 times (w / v, g / mL) of petroleum ether to the crude product of sucrose-6-acetate prepared by the dibutyltin oxide method, stir vigorously to form an emulsion, and then mix with 3 times (w / w ) coarse-pore silica gel (200-400 mesh) and mix well, put it into the above-mentioned silica gel column, and fill it to about 4 / 5 of the height of the chromatography column.

[0031] Rinse the column with a mixed solution of petroleum ether and dichloromethane (v / v=90:10), discard the fraction without sucrose-6-acetate, and start collecting when sucrose-6-ac...

Embodiment 3

[0033] Inject 2 / 3 of the volume of petroleum ether into the 1.5m-high chromatographic column, and put in coarse-pore silica gel (200-300 mesh) from the feeding port to about 3 / 5 of the height of the chromatographic column, stir while pouring, and then statically Set for about 3h. Open the outlet valve to lower the liquid level of petroleum ether in the chromatography column to 5-10 cm above the top surface of the silica gel.

[0034] Add about 1 times (w / v, g / mL) petroleum ether to the crude sucrose-6-acetate, stir vigorously to form an emulsion, and then mix with 1 times (w / w) coarse-porous silica gel (200~300 mesh) and mix evenly, put it into the above-mentioned silica gel column, and fill it to about 4 / 5 of the height of the chromatographic column.

[0035] Rinse the column with a mixed solution of petroleum ether and ethyl acetate (v / v=10:1), discard the fraction without sucrose-6-acetate, and start collecting when sucrose-6-acetate is precipitated. Until the end of sucr...

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Abstract

The invention discloses a purification method for sucrose-6-acetate, which belongs to the technical field of purification of organic matters. The method comprises the following steps: mixing a crude product of sucrose-6-acetate with petroleum ether to form an emulsion; uniformly mixing the emulsion with silica gel to form a to-be-separated liquid; and adding the to-be-separated liquid into a silica gel-petroleum ether chromatographic column for chromatographic separation by using a developing solvent and subjecting a flow containing sucrose-6-acetate to reduced pressure condensation so as to obtain a finished product of sucrose-6-acetate. The purification method for sucrose-6-acetate provided by embodiments in the invention has the advantages of simple process, high purity (more than 98%) and high yield of the target product, capacity of improving purity and quality of the final product sucralose and reduced production cost. Since the developing solvent and the silica gel used in the process of separation can be reused, cost for purification is effectively reduced.

Description

technical field [0001] The invention belongs to the technical field of organic matter purification, in particular to a method for purifying sucrose-6-acetate. Background technique [0002] Sucralose is currently found to be the most suitable high-efficiency sweetener for human use. In its industrial preparation process, the intermediate sucrose-6-acetate must first be obtained. So far, there are two main methods of producing sucrose-6-acetate that are truly industrially valuable: [0003] In the patent No. US4889928 and US5449772, a method for the synthesis of sucrose-6-acetate by trimethyl orthoacetate method is disclosed. ) in a solvent with p-toluenesulfonic acid as a catalyst for ring closure reaction, adding water to open the ring, and finally adding tert-butylamine to complete the transposition reaction, and concentrating under reduced pressure to obtain sucrose-6-acetate. [0004] The patent No. US4950746, US5023329 discloses a method for synthesizing sucrose-6-acet...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H13/06C07H1/06
Inventor 梁恒波段小六
Owner HUBEI HONGYUAN PHARMA
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