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Method for preparing sucralose-6-ester by utilizing bis(trichloromethyl)carbonate

A technology of sucralose and solid phosgene, applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of difficult separation, reduced utilization value, high absorption cost, etc., and achieve the effect of reducing cost input

Inactive Publication Date: 2015-12-02
SHANDONG KANBO BIOCHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 1) The tail gas is a mixed gas of a large amount of sulfur dioxide and hydrogen chloride, and the two are not easy to be completely separated. The by-product hydrochloric acid contains sulfur, which greatly reduces its utilization value. The absorption cost of sulfur dioxide gas with liquid alkali is relatively high, and the by-product sodium sulfite contains sodium chloride. and other impurities also greatly reduce its utilization value

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: A kind of preparation method that utilizes solid phosgene to carry out sucralose 6 ethyl ester that the present invention mentions, comprises the following steps:

[0020] 1) Prepare 6-ethyl sucrose by monoester method, the content is about 75%, the mass of sucrose input is 40 grams, and the obtained esterification solution is 139.52 g;

[0021] 2) Put 100.34 grams of solid phosgene and 600 grams of trichloroethane into a 1000 mL four-neck flask, stir to dissolve, and cool down to -5 °C in an ice-salt water bath;

[0022] 3) Add sucrose 6 ethyl ester dropwise, and control the temperature below 5°C;

[0023] 4) Keep warm at 0-5°C for 2 hours, then raise the temperature to 115°C, and keep warm for 2 hours;

[0024] 5) At the end of the heat preservation, lower the temperature to 0°C, add ammonia water dropwise to adjust the pH value to 10, stir for 5 minutes and add hydrochloric acid dropwise to adjust the pH value to 7.

[0025] 6) Distill under reduced p...

Embodiment 2

[0027] Embodiment 2: A kind of preparation method that utilizes solid phosgene to carry out sucralose 6 ethyl ester that the present invention mentions, comprises the following steps:

[0028] 1) Prepare sucrose 6 ethyl ester by monoester method, the content is about 75%, the mass of sucrose input is 40 grams, and the obtained esterification solution is 139.28g;

[0029] 2) Put 102 grams of solid phosgene and 600 grams of trichloroethane into a 1000 mL four-neck flask, stir to dissolve, and cool down to -5 °C in an ice-salt water bath;

[0030] 3) Add sucrose 6 ethyl ester dropwise, and control the temperature below 5°C;

[0031] 4) Keep warm at 0-5°C for 2 hours, then raise the temperature to 115°C, and keep warm for 2 hours;

[0032] 5) At the end of the heat preservation, lower the temperature to 0°C, add ammonia water dropwise to adjust the pH value to 10, stir for 5 minutes and add hydrochloric acid dropwise to adjust the pH value to 7.

[0033] 6) Distill under reduced...

Embodiment 3

[0035] Embodiment 3: A kind of preparation method that utilizes solid phosgene to carry out sucralose 6 ethyl ester that the present invention mentions, comprises the following steps:

[0036] 1) Prepare sucrose 6 ethyl ester by monoester method, the content is about 75%, the mass of sucrose input is 40 grams, and the obtained esterification liquid is 138.22g;

[0037] 2) Put 102 grams of solid phosgene and 600 grams of trichloroethane into a 1000 mL four-neck flask, stir to dissolve, and cool down to -5 °C in an ice-salt water bath;

[0038] 3) Add sucrose 6 ethyl ester dropwise, and control the temperature below 5°C;

[0039] 4) Keep warm at 0-5°C for 2 hours, then raise the temperature to 115°C, and keep warm for 2 hours;

[0040] 5) At the end of the heat preservation, lower the temperature to 0°C, add ammonia water dropwise to adjust the pH value to 10, stir for 5 minutes and add hydrochloric acid dropwise to adjust the pH value to 7.

[0041] 6) Distill under reduced p...

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PUM

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Abstract

The invention relates to a method for preparing sucralose-6-ester by utilizing bis(trichloromethyl)carbonate. The method comprises the following steps: 1) reacting sucrose to obtain an esterification liquid; 2) adding bis(trichloromethyl)carbonate and trichloroethane to a reaction kettle, stirring the materials to dissolve the materials until the liquid is clear, and reducing the temperature with an ice brine bath; 3) slowly dropwise adding a dimethylformamide solution of sucrose-6-ester to the reaction kettle; 4) maintaining the temperature below 5 DEG C for 2 hours after dropwise adding is completed; 5) carrying out programmed temperature raising and maintaining; 6) reducing the temperature, adjusting the pH value to 10, stirring the solution and adjusting the pH value to 7; 7) removing the trichloroethane solvent, adding water, carrying out suction filtration, weighing the filter residues and computing the yield. The method has the beneficial effects that 1) the tail gases are absorbed only with water, so that the method has the advantages that the cost input is reduced, the byproduct hydrochloric acid is purer, the color is transparent and the value in use is higher compared with existing water absorption and sodium hydroxide absorption methods; and 2) liquid chromatographic analysis verifies that the yield of a bis(trichloromethyl)carbonate method is 60%, and the yield of a thionyl chloride method is 55%.

Description

technical field [0001] The invention relates to a preparation method of sucralose 6 ethyl ester, in particular to a preparation method of sucralose 6 ethyl ester by using solid phosgene. Background technique [0002] The industrial production of sucralose is mainly divided into three parts: the synthesis of sucralose 6 ethyl ester by monoester method, the synthesis of sucralose 6 ethyl ester by thionyl chloride method, and the preparation of sucralose by alcoholysis of sodium methoxide. Among them, the process of synthesizing sucralose 6 ethyl ester by thionyl chloride method brings two big problems: [0003] 1) Tail gas is a mixed gas of a large amount of sulfur dioxide and hydrogen chloride, and the two are not easy to be completely separated. The by-product hydrochloric acid contains sulfur, which greatly reduces its utilization value. The absorption cost of sulfur dioxide gas with liquid alkali is high, and the by-product sodium sulfite contains sodium chloride. And oth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H13/06C07H1/00C07H1/06
Inventor 李建新李建彬徐松波
Owner SHANDONG KANBO BIOCHEM TECH
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