Chlorination method for industrial production of sucralose-6-acetic ester

A technology of sucralose and acetate, applied in chemical instruments and methods, esterified saccharides, sugar derivatives, etc., can solve the problems of low reaction yield and conversion rate of thionyl chloride, and reduce separation Burden, increase conversion rate, easy to operate effect

Active Publication Date: 2011-07-13
JK SUCRALOSE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, when using thionyl chloride, because a large amount of product gases are dissolved in the reaction solution, from the perspective of reaction balance, the conversion rate will inevitably decrease.
This may be another important reason why the yield of thionyl chloride reaction is lower than that of phosgene

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1: To 100 kg of sucrose-6-acetate dry syrup (converted to 100% of sucrose-6-acetate), add 180 kg of N,N-dimethylformamide, and add 1100 after homogenization Liter 1,1,2-trichloroethane. The temperature was lowered to -15°C, and 300 kg of thionyl chloride was added with stirring and kept at -15°C. The temperature is raised to room temperature and kept for 1 hour; the temperature is raised to 70°C in 1 hour and the temperature is kept for 0.5 hours; the temperature is raised to 100°C in 1 hour and the temperature is kept for 2 hours; the temperature is raised to reflux for 2 hours and the reaction is completed. After neutralization, solvent removal, water dissolution, decolorization, crystallization, etc., 85 kg of crude sucralose-6-acetate product was obtained.

Embodiment 2

[0019] Example 2: 120 kg of sucrose-6-acetate dry syrup (converted to 100% sucrose-6-acetate content), add 160 kg of N,N-dimethylformamide, add 1200 liters after homogenization Toluene. The temperature was lowered to -15°C, and 260 kg of thionyl chloride was added with stirring and kept at -15°C. The temperature is increased to room temperature and the temperature is maintained for 1 hour; the temperature is increased to 70°C in 1.5 hours and the temperature is maintained for 0.5 hours; the temperature is increased to 100°C in 1.5 hours and the temperature is maintained for 2 hours; the temperature is refluxed for 2.5 hours and the reaction is completed. After neutralization, solvent removal, water dissolution, decolorization and crystallization, 104 kg of crude sucralose-6-acetate product was obtained.

Embodiment 3

[0020] Example 3: 100 kg of sucrose-6-acetate dry syrup (converted to 100% sucrose-6-acetate content), add 160 kg of N,N-dimethylformamide, add 1100 liters after homogenization Toluene. The temperature was lowered to -15°C, and 260 kg of thionyl chloride was added with stirring and kept at -15°C. The temperature is raised to room temperature and kept for 1 hour; the temperature is raised to 70°C in 1.5 hours and the temperature is kept for 0.5 hours; the temperature is raised to 100°C in 1.5 hours and the temperature is kept for 2 hours; the temperature is raised to 113°C in 1.5 hours and the temperature is kept for 2 hours. The reaction is over. After neutralization, desolventization, water dissolution, decolorization, crystallization, etc., 79 kg of crude sucralose-6-acetate product was obtained.

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PUM

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Abstract

The invention discloses a chlorination method for industrial production of sucralose-6-acetic ester and relates to the chlorination method for industrial production of the sucralose-6-acetic ester which is a key intermediate of sucralose. The method specifically comprises the steps of adding 7-11 times of molar ratio of N, N-dimethylformamide into pre-synthesized sucrose-6-acetic ester solid or dry syrup, carrying out homogenization, dissolving in 2-6 times of volume ratio of organic solvent, dripping thionyl chloride with molar weight which is equal to that of N, N-dimethylformamide below 0 DEG C, generating a vilsmeier reagent, stirring, naturally increasing the temperature to room temperature, further using 2-14 hours for slowly increasing the temperature to 110-115 DEG C, keeping the temperature for 1-3 hours at 110-115 DEG C, and carrying out neutralization, solvent removal, dissolution by adding water, decolorization and crystallization after the completion of reaction, so as toobtain a sucralose-6-acetic ester coarse product. The method has the advantages of high yield, simple operation, convenient post-treatment and ability of being applicable to industrial production.

Description

Technical field [0001] The invention relates to a new chlorination method for industrial production of sucralose, a key intermediate sucralose-6-acetate. Background technique [0002] Sucralose-6-acetate is a key intermediate in the production process of sucralose. It is prepared by the chlorination reaction of sucrose-6-acetate with chlorinating reagents under suitable conditions. There are usually two types of chlorination reagents reported in the literature: one is vilsmeier chlorination reagent (USP 4980463), and the other is thionyl chloride / pyridine / chlorinated hydrocarbon ternary chlorination system (USP 5136031). According to many reasons such as clear reaction mechanism, cheap and easy-to-obtain raw materials, stable process operation, and convenient solvent separation and recovery, most domestic sucralose production enterprises and the British Taylor company use the first type of vilsmeier chlorinating reagent as the chlorination agent. Reaction raw materials. [0003] ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H13/06C07H1/00
Inventor 吴金山朱国廷安立军陈宜武
Owner JK SUCRALOSE
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