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Synthesis method of sucrose-6-acetate

A synthetic method and acetate technology, applied in the direction of chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve the problems of low yield, low product purity, complicated process, etc., and achieve high yield and high product quality. The effect of high purity

Inactive Publication Date: 2010-04-14
李松伦
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the present open technology, the preparation method of sucrose-6-acetate mainly contains two kinds: the ethyl acetate method described in US4889928 and the dibutyltin oxide method described in US4950746, these methods have certain advancement, but There are disadvantages such as complex process, low yield and low product purity

Method used

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Examples

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Effect test

Embodiment 1

[0013] In a 1000ml three-necked flask, add 50g of sucrose, 250ml of dimethylformamide, 3g of potassium carbonate and 2g of benzyltriethylamine chloride, heat until dissolved, then cool to below room temperature, and add 60ml of ethyl acetate dropwise to react; After the ethyl acetate was added dropwise, the temperature was raised to 80°C to continue the reaction for 4 hours, cooled to room temperature, the catalyst was removed by filtration, unreacted ethyl acetate was distilled off, and dimethylformamide was distilled off under reduced pressure to obtain 57 g of the product. As detected by HPLC, the content of sucrose-6-acetate was 85.3%.

Embodiment 2

[0015] In a 1000ml three-necked flask, add 50g of sucrose, 280ml of dimethyl sulfoxide, 2g of sodium carbonate and 3g of benzyltriethylamine chloride, heat to dissolve, then cool to below room temperature, and add 70ml of ethyl acetate dropwise to react; After the ethyl acetate was added dropwise, the temperature was raised to 90°C to continue the reaction for 3 hours, cooled to room temperature, the catalyst was removed by filtration, unreacted ethyl acetate was distilled off, and then dimethylformamide was distilled off under reduced pressure to obtain 58 g of the product. As detected by HPLC, the content of sucrose-6-acetate was 82.6%.

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PUM

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Abstract

The invention discloses a synthesis method of sucrose-6-acetate, which is characterized by comprising the following steps: adding a solvent in sucrose as raw material, heating until dissolving the sucrose under the action of carbonate as a catalyst and benzyltriethylammonium chloride as a phase transfer catalyst; then cooling to be below room temperature, dropwise adding ethyl acetate for reaction; after the ethyl acetate is added, raising the temperature to 60-95 DEG C; continuously reacting for 2-6h, cooling to room temperature; filtering to remove the catalyst; and distilling over unreacted ethyl acetate to obtain the sucrose-6-acetate. The invention has the advantages of simple process, easy operation, high yield and high product purity.

Description

technical field [0001] The invention relates to a synthesis method with simple process but capable of obtaining high-purity sucrose-6-acetate. Background technique [0002] Sucralose is a functional sweetener, which represents the latest achievement in the development of sweeteners, and its chemical name is 4,1',6-trichloro-4,1',6'-trideoxygalactosucrose , the three hydroxyl groups 4, 1, and 6 in the molecule are replaced by three oxygen atoms; and there are eight hydroxyl groups in the sucrose molecule, which are three primary carbon hydroxyl groups (6, 1', 6' positions) and five secondary Carbon hydroxyl group (2, 3, 4, 3', 4' position), if sucralose is to be prepared, the 6-position hydroxyl group must be protected. [0003] In the present disclosed technology, the preparation method of sucrose-6-acetate mainly contains two kinds: the ethyl acetate method described in US4889928 and the dibutyltin oxide method described in US4950746, these methods have certain advancement...

Claims

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Application Information

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IPC IPC(8): C07H13/06C07H1/00
Inventor 李松伦
Owner 李松伦
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