Method for preparing-ester by using solid chlorine substitution of phosgene

A technology for solid phosgene and sucralose, applied in the field of sucralose-6-ester preparation, can solve the problems of unsuitable storage and transportation, side reactions, inconvenience and accurate measurement, etc., and achieves avoiding side reactions, low toxicity, reducing Effects of waste gas treatment steps and equipment requirements

Active Publication Date: 2005-08-31
JK SUCRALOSE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the yield of phosgene is high, phosgene is a highly toxic gas, which is not suitable for storage and transportation. At the same time, it is not convenient to measure phosgene accurately as a gas, especially when the laboratory needs a small amount of accurate quantitative phosgene, excessive use prone to side effects

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Embodiment 1: 10 grams of sucrose-6-acetates are dissolved in 90 milliliters of dimethylformamide, slowly add the toluene solution of solid phosgene (containing 25 grams of solid phosgene) at -10 ℃, the reaction mixture remains low Stir vigorously at 5°C for 0.5 hours. Then the temperature was raised to 115° C. over 2.5 hours and maintained for 4 hours. After the reaction product is cooled to room temperature, it is neutralized by an inorganic base or an organic base, the solvent is removed by distillation, dissolved in water, decolorized by activated carbon, extracted from the organic phase (the extracted organic solvent is ethyl acetate), and crystallized to obtain sucralose-6-ester Product, the product was analyzed by HPLC and showed that the yield of sucralose-6-ester was 62.2%.

Embodiment 2

[0012] Example 2: 8 grams of sucrose-6-acetate was dissolved in 70 milliliters of dimethylformamide, and a dichloromethane solution of solid phosgene (containing 18 grams of solid phosgene) was added dropwise in an ice-salt bath. The reaction mixture was kept below 5°C and stirred vigorously for 0.5 hours. Then the temperature was raised to 115° C. over 3.5 hours and kept for 4 hours. A trap collects the condensed methylene chloride. After the reaction, the product is cooled to room temperature, neutralized by an inorganic base or an organic base, the solvent is removed by distillation, dissolved in water, decolorized by activated carbon, extracted with an organic solvent (the extracted organic solvent is ethyl acetate), and crystallized to obtain sucralose-6- The ester product, HPLC showed that the yield of sucralose-6-ester was 58.3%.

Embodiment 3

[0013] Example 3: 5 grams of sucrose-6-acetate was dissolved in 60 milliliters of dimethylformamide, and a solution of solid phosgene in carbon tetrachloride (containing 10 grams of solid phosgene) was added dropwise at -10°C. The reaction mixture was kept below 5°C and stirred vigorously for 0.5 hours. Then the temperature was raised to 113° C. over 3.5 hours and kept for 3 hours. After the reaction, the product was cooled to room temperature, neutralized with alkaline solution, distilled to remove the solvent, dissolved in water, decolorized with activated carbon, extracted with an organic solvent (the extracted organic solvent was ethyl acetate), and crystallized to obtain the sucralose-6-ester product, HPLC The yield of sucralose-6-ester was shown to be 56.7%.

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Abstract

A process for preparing trichlorosucrose-6-ester by solid-state phosgene chlorinating includes dissolving solid phosgene in inertial solvent, slowly dropping it in the solution of sucrose-6-ester in dimethyl formamide, stirring, heating while reaction, alkali solution neutralizing, distilling to remove solvent, dissolving in water, decoloring by activated carbon, extracting in organic solvent and crystallizing.

Description

technical field [0001] The invention relates to a method for preparing sucralose-6-ester with solid phosgene [bis(trichloromethyl)carbonate] chlorosucrose-6-ester, belonging to the technical field of sucralose-6-ester preparation . Background technique [0002] Sucralose (4,1',6'-trichloro-4,1',6'-trideoxygalactosucrose) is a low-energy strong sweetener with high sweetness, good sweetness, With the characteristics of good acid hydrolysis stability, low calorific value, non-toxicity, and anti-caries, it is one of the most ideal sweeteners that can be seen in the European and American markets. [0003] Sucralose is a product in which the three hydroxyl groups at the 4-, 1'- and 6'-positions of the sucrose molecule are replaced by chlorine atoms. There are 8 hydroxyl groups in the sucrose molecule, including 3 primary hydroxyl groups (6-, 1'-, 6'-) and 5 secondary hydroxyl groups (2-, 3-, 4-, 3'-, 4'-) , Their chemical reactivity is quite different,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H13/02
Inventor 沈彬陆正清张满宋爱平傅颖红
Owner JK SUCRALOSE
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