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Preparation method for sucrose trichloride -2,3,6,3',4'-pentaacetate

A technology of pentaacetate and sucralose, applied in the directions of food preparation, chemical instruments and methods, sugar derivatives, etc., can solve problems such as residues, increase production costs, increase post-processing procedures of finished products, etc., and achieve mild reaction process conditions. Effect

Inactive Publication Date: 2012-03-21
CHANGZHOU NIUTANG CHEM PLANT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Looking at the above methods, there are problems: 1, the raw material triphenylphosphine oxide is expensive and does not meet the actual production needs; 2, triphenylphosphine oxide is highly toxic and will remain in the finished product, thereby increasing the post-treatment process of the finished product and increasing Cost of production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A 1000ml four-neck round-bottom flask equipped with mechanical stirring, thermometer and condenser tube was added with 700ml DMF containing 100g (0.18mol) sucrose-2,3,6,3',4'-pentaacetate (N,N -Dimethylformamide) solution, cooled to -10~0°C, added dropwise 100g (0.84mol) thionyl chloride, kept warm for half an hour after the dropwise addition, then slowly raised the temperature to 110-115°C within 1 hour, kept React for 3 hours; after the reaction is over, cool to room temperature, adjust the pH to neutral with liquid caustic soda, then extract three times with 200ml ethyl acetate, decolorize with activated carbon, concentrate to remove ethyl acetate, add 150ml of water, heat to dissolve, then cool to precipitate crystals , suction filtration, and drying to obtain 91.6 g of sucralose-2,3,6,3',4'-pentaacetate crystals with a purity of 98.5% (HPLC) and a yield of 83.4%.

Embodiment 2

[0026] A 1000ml four-neck round-bottomed flask equipped with mechanical stirring, thermometer and condenser tube was added with 700ml DMF solution containing 100g (0.18mol) sucrose-2,3,6,3',4'-pentaacetate and cooled to -20~-10°C, add 110g (0.92mol) thionyl chloride dropwise, keep warm for half an hour after the dropwise addition, then slowly raise the temperature to 110-115°C within 1 hour, keep warm for 4 hours; after the reaction is over, cool to At room temperature, use liquid caustic soda to adjust the pH to neutral, and then extract three times with 200ml ethyl acetate, decolorize with activated carbon, concentrate to remove ethyl acetate, add 150ml water, heat to dissolve, cool to precipitate crystals, filter with suction, and dry to obtain 85.5g three Sucralose-2,3,6,3',4'-pentaacetate crystals, with a purity of 98.0% (HPLC), and a yield of 77.8%.

Embodiment 3

[0028] A 1000ml four-neck round-bottomed flask equipped with mechanical stirring, thermometer and condenser tube was added with 700ml DMF solution containing 100g (0.18mol) sucrose-2,3,6,3',4'-pentaacetate and cooled to -25~-15°C, add 90g (0.75mol) thionyl chloride dropwise, keep warm for half an hour after the dropwise addition, then slowly raise the temperature to 110-115°C within 1 hour, keep warm for 2 hours; after the reaction is over, cool to At room temperature, use liquid caustic soda to adjust the pH to neutral, then extract three times with 200ml ethyl acetate, decolorize with activated carbon, concentrate to remove ethyl acetate, add 150ml water, heat to dissolve, cool to precipitate crystals, filter with suction, and dry to obtain 82.6g three Chlorose-2,3,6,3',4'-pentaacetate crystals, the purity is 97.6% (HPLC), and the yield is 75.1%.

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Abstract

The present invention relates to a method for preparing sucralose-2, 3, 6, 3', 4'-pentaacetate. Sucrose-2, 3, 6, 3', 4'-pentaacetate is added into solvent containing tertiary amine, and after the temperature is decreased to 0 DEG C, thionyl chloride is dripped in; then, after being increased to 110 DEG C to 115 DEG C, the temperature is kept for two to six hours; after sufficient reaction, the temperature is reduced to the room temperature; caustic soda liquid is used to carry out neutralization; ethyl acetate is used to carry out extraction and condensation; water is added into the extract and heated until the extract is resolved; and sucralose-2, 3, 6, 3', 4'-pentaacetate crystals are precipitated by cooling. Compared with the prior art, the technical scheme of the method has the advantages of mild reaction conditions and easy control, and both the yield and purity of the product are higher than the optimal values of the prior art.

Description

technical field [0001] The present invention relates to the food sweetener "sucralose", especially to the preparation method of the key intermediate "sucralose-2,3,6,3',4'-pentaacetate" of the food sweetener , belonging to the field of fine chemical technology. Background technique [0002] Sucralose is a functional sweetener, and to some extent it represents the latest achievement in the development of sweeteners. From the molecular structure, it is the 4, 1', 6' three hydroxyl groups in the sucrose molecule. replaced by three chlorine atoms. There are 8 hydroxyl groups in the sucrose molecule, which are three primary carbon hydroxyl groups (6, 1', 6' positions) and five secondary carbon hydroxyl groups (2, 3, 4, 3', 4' positions). Chlorose, one method is to protect the 6-hydroxyl in the sucrose molecule, and then perform selective chlorination. Since the 1' and 6'-hydroxyls are primary hydroxyl groups, they are relatively active, and the chlorination reaction is easy to ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H13/06A23L1/236A23L27/30
Inventor 王方大蔡亚高正兵陈凯
Owner CHANGZHOU NIUTANG CHEM PLANT CO LTD
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