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Method for preparing sweetening agent sucralose by one-pot process

A technology of sucralose and sucrose, which is applied to the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of difficult intermediate product purification, complicated operation process, and inconvenient operation, and achieve the improvement of industrial production level, The process is simple and environmentally friendly, and the effect of reducing wastewater discharge

Active Publication Date: 2015-01-21
XINFA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the domestic production of sucralose is low, and most of them depend on imports, which leads to the fact that sucralose is only used in high-end foods and not widely used
[0007] The preparation methods of sucralose mainly include tritylation method, monoesterification method, chlorination method of sucrose derivatives, biological method and cottonseed triose method. The above methods have many synthesis steps, complicated process flow, cumbersome chemical and enzymatic fermentation and Difficult to purify intermediates
In the acylation reaction of this technical scheme, ketene gas is used as the acetylation reagent, and ketene is a dangerous raw material, which is inconvenient to operate
And the three-step operation process of acylation, chlorination and hydrolysis is complicated, which is not conducive to industrial production

Method used

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  • Method for preparing sweetening agent sucralose by one-pot process
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  • Method for preparing sweetening agent sucralose by one-pot process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Under nitrogen protection, 200 g of N,N-dimethylformamide, 34.2 g (0.1 mol) of sucrose, and 0.14 g of p-toluenesulfonic acid were sequentially added to a dry 1000 ml glass flask. Keep at 0°C-10°C, add 2.31g (0.034mol) boric anhydride in batches, keep warm at 10°C-20°C for 3 hours, liquid phase detection of sucrose conversion is complete; then cool in ice water, keep at 0°C-10°C, add dropwise 39.3 grams (0.33 moles) of thionyl chloride, after dropping, the reaction was heated up in stages, stirred at 20°C to 30°C for 2 hours, 70°C to 90°C for 2 hours, 120°C to 150°C for 3 hours, About 150 g of solvent was recovered by distillation under reduced pressure, and cooled to room temperature. Add 120 grams of saturated sodium chloride aqueous solution, stir and hydrolyze at room temperature for 3 hours; add ethyl acetate for extraction three times, share 130 grams of ethyl acetate, combine the organic phases, wash twice with 30 grams of saturated sodium chloride aqueous solutio...

Embodiment 2

[0045] As described in Example 1, the difference is that the acid catalyst is selected from methanesulfonic acid, and 80 mg of methanesulfonic acid is used to replace 0.14 gram of p-toluenesulfonic acid in Example 1 to react, and the preparation steps and conditions are the same as in the implementation Example 1, the resulting product purity and yield are shown in Table 1.

Embodiment 3

[0047] As described in Example 1, the difference is that the acidic catalyst is selected from 98% vitriol oil, and 80 mg of 98% vitriol oil is used to replace 0.14 gram of p-toluenesulfonic acid in Example 1 to react, and the preparation steps and conditions are the same as in the implementation Example 1, the resulting product purity and yield are shown in Table 1.

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Abstract

The invention relates to a method for preparing a sweetening agent sucralose by a one-pot process. The method comprises the following steps of: protecting sucrose which is taken as a raw material by sucrose-6-hydroxyl through boron anhydrous with presence of an acid catalyst and a solvent, directly implementing a chlorination through thionyl chloride without separating disucrose borate which is an intermediate product to obtain hexachloro disucrose borate, and hydrating to obtain the sucralose. The method disclosed by the invention sequentially implements three reactions, namely selective protection, chloro reaction and hydration, of the sucrose-6-hydroxyl in one pot to prepare the sucralose, and the process is simple and convenient and reduces discharge of wastewater; and the prepared sucralose product is high in purity, high in yield, low in cost, and suitable for industrial production.

Description

technical field [0001] The invention relates to a production method of sweetener sucralose, in particular to a method for preparing sucralose by using boric anhydride one-pot method, and belongs to the technical field of food additive production. Background technique [0002] Sucralose (Trichlorosucrose) is a halogenated sucrose derivative with the chemical name 1′,6′-dichloro-1′,6′-dideoxy-β-D-fructofuranose-4-chloro-4-deoxy -2-D-fructopyranose was developed by British Tate & Lyle and Professor Hough L of the University of London. In 1976, a patent application for a new type of sweetener was filed. The structural formula of sucralose is as follows: [0003] [0004] Sucralose [0005] The taste of sucralose is mellow and rich, very close to sucrose, the sweetness characteristic curve almost overlaps with sucrose, without any bitterness, and the sweetness can reach 600 times of sucrose. Sucralose is a white crystalline powder with a melting point of 130 deg...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H5/02C07H1/00
Inventor 戚聿新陈军王世明牛伟李新发
Owner XINFA PHARMA
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