Chlorination method for trichlorosucrose preparation

A technology of sucralose and chlorinating reagents, applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve the problems of reducing sweetness compounds, complex synthesis processes, etc., achieving easy operation control, broad development and Application prospect and effect of energy saving

Inactive Publication Date: 2008-08-13
江建成
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its early synthesis process is very complicated, because the reactivity of its hydroxyl functional group in the sucrose molecule is 6, 6' > 4 > 1' > other

Method used

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  • Chlorination method for trichlorosucrose preparation
  • Chlorination method for trichlorosucrose preparation
  • Chlorination method for trichlorosucrose preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] A method for chlorination in the preparation of sucralose, the process steps are as follows:

[0047] 1. At room temperature, put 600ml of N,N-dimethylformamide in a 2000ml reaction vessel, slowly add 180ml of thionyl chloride under normal temperature stirring conditions, the temperature is not easy to rise too fast, a better method is to put it under the reaction vessel (Natural) water, after the dropwise addition is completed, stir for 1-2 hours, then slowly add 300 grams (100 grams of equivalent sugar) sucrose-6-acetate dropwise under normal temperature conditions, heat up immediately after the end, and 80°C, 100°C, 113°C for 1 hour, 1.5 hours, 2-2.5 hours respectively, and should not exceed 115°C;

[0048] 2. After the segmental heating is completed, stir and cool to room temperature, add about 600 grams of 31% concentrated NaOH solution dropwise at room temperature until the pH is about 9, stir for about half an hour and reverse the adjustment of about 70 grams of ...

Embodiment 2

[0052] A method for chlorination in the preparation of sucralose, the process steps are as follows:

[0053] 1. At room temperature, put 700ml of N,N-dimethylformamide in a 2000ml reaction vessel, slowly add 180ml of thionyl chloride under normal temperature stirring conditions, the temperature is not easy to rise too fast, a better method is to put it under the reaction vessel (Natural) water, after the dropwise addition is completed, stir for 1-2 hours, then slowly add 300 grams (100 grams of equivalent sugar) sucrose-6-acetate dropwise under normal temperature conditions, heat up immediately after the end, and 80°C, 100°C, 113°C for 1 hour, 1.5 hours, 2-2.5 hours respectively, and should not exceed 115°C;

[0054] 2. After the segmental heating is completed, stir and cool to room temperature, and add about 750 grams of 31% concentrated NaCO dropwise at room temperature. 3 Solution until the pH is about 9, stir for about half an hour and reverse 70 grams of 32% concentrated...

Embodiment 3

[0058] A method for chlorination in the preparation of sucralose, the process steps are as follows:

[0059]1. At room temperature, put 900ml of N,N-dimethylformamide in a 2000ml reaction vessel, slowly add 180ml of thionyl chloride under normal temperature stirring conditions, the temperature is not easy to rise too fast, a better method is to put it under the reaction vessel (Natural) water, after the dropwise addition is completed, stir for 1-2 hours, then slowly add 300 grams (100 grams of equivalent sugar) sucrose-6-acetate dropwise under normal temperature conditions, heat up immediately after the end, and 80°C, 100°C, and 113°C for 1 hour, 1.5 hours, and 2-2.5 hours respectively, and should not exceed 115°C;

[0060] 2. After the segmental heating is completed, stir and cool to room temperature, add about 255 grams of 31% concentrated ammonia water dropwise at room temperature until the pH is about 9, and stir for about half an hour to reverse adjust about 70 grams of 3...

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Abstract

The invention discloses a chlorination process in preparation of sucralose, including steps of: putting N,N-dimethylformamide into reaction vessels, adding chlorination agent at normal temperature, wherein ratio between chlorination agent and N,N-dimethylformamide is in range of 1:2.5-7.5 (mol ratio), adding sucrose-6-acetate, heating directly while controlling temperature, adding thick sodium hydroxide for neutralisation in normal temperature after reaction, adding organic solution group by group for extraction after a after-treatment; treating organic facies, and refining subsequently so that chlorid of sucralose is obtained. The process is characterized by mild reacting condition, easiness to control, and low energy consumption, thus has a great expectation for development and application.

Description

technical field [0001] The invention belongs to the field of fine chemical industry and relates to an artificially synthesized food additive-sucralose, in particular to a chlorination method in the preparation of sucralose. Background technique [0002] 1.1. Structure and characteristics of sucralose [0003] Sucralose, also known as sucralose, has a chemical name of 4,1',6'-trichloro-4,1',6'-trideoxygalactose, which is synthesized from sucrose. Its chemical structure is as [0004] [0005] Sucralose is currently the product of the highest level of research and development of high-intensity sweeteners in the world, with excellent performance. Compared with other high-intensity sweeteners, sucralose has the following advantages: [0006] 1) High sweetness, 600-800 times that of sucrose; [0007] 2) The sweetness is pure, without any peculiar smell or bitterness, and the sweetness characteristic curve almost overlaps with that of sucrose; [0008] 3) Safe, non-toxic, n...

Claims

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Application Information

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IPC IPC(8): C07H5/02
Inventor 江建成荣先冬
Owner 江建成
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