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Methods for extracting and purifying sucralose intermediate

A technology for extracting sucralose and sucralose, which is applied in the field of extraction and purification of sucralose intermediates, and can solve the problems of expensive production time and cost

Inactive Publication Date: 2011-08-24
MAMTEK INT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the sucralose production method using this esterification method is expensive in terms of raw materials, equipment, and production time
And the use of acetic anhydride, pyridine, and toluene can create various environmental and health concerns

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0029] Sucrose-6-acetate was prepared using 34 grams of sucrose, which was then reacted with triphosgene. The pH of the reaction mixture was adjusted first to 8-9 and then to 6-7. The reaction mixture was heated to 65°C with a water bath and dried at -0.098 MPa. The dried sucralose intermediate was redissolved in 200 mL of water and filtered. The aqueous solution was extracted with ethyl acetate (200 mL, 6x), and the ethyl acetate fractions were combined.

[0030] The combined ethyl acetate fraction was dried at -0.098 MPa and 35°C. The dried material was redissolved in 50 ml of water. To this aqueous solution was added 50 mL of ether to precipitate sucralose-6-acetate which was filtered and collected. Yield: 15-18 g of semi-purified sucralose-6-acetate.

[0031] The semi-purified sucralose-6-acetate was redissolved in 2.5 times (volume to weight) ethyl acetate at 60°C. The ethyl acetate solution of sucralose-6-acetate was cooled slowly. After 6 hours, the sucralose-6-a...

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PUM

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Abstract

The present invention provides a method for purifying sucralose-6-ester for use in making sucralose, wherein the method eliminates the need of an esterification process. In particular, ethyl acetate and ether are used to extract and purify sucralose-6-ester from a sucralose production intermediate composition comprising sucralose-6-ester.

Description

technical field [0001] The present invention generally relates to methods for the extraction and purification of sucralose intermediates, particularly sucralose-6-ester. Background technique [0002] The artificial sweetener 4,1',6'-trichloro-4,1',6'-trideoxygalactosucrose ("sucralose") is produced by replacing the 4,1', and 6' positions with chlorine The hydroxyl group is derived from sucrose. A number of different synthetic routes have been developed for the preparation of sucralose, in which the reactive hydroxyl group at the 6-position is blocked with an ester group and then hydrolyzed to remove Ester substituents, resulting in sucralose. Some of these synthetic routes involve tin-mediated sucrose-6-ester synthesis. [0003] Sucrose-6-ester can be chlorinated, eg, by the method of Walkup et al. (US Patent No. 4,980,463, which is hereby incorporated by reference in its entirety). Products produced by this chlorination process include solutions of sucralose-6-esters su...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/06C07H3/00C07H1/00
CPCC07H13/04C07H13/08C07H3/00C07H1/06C07H1/00
Inventor 戴维·乐三·何万正豪
Owner MAMTEK INT