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Synthetic method for sucralose

A technology for sucralose and a synthesis method, applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve the problems of long cycle, difficult purification, low conversion rate, etc., and achieves ingenious methods, mild crystallization, and reduced cost effect

Inactive Publication Date: 2011-08-31
李罡
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And the existing sucrose-6-ester reaction uses triethyl orthoformate for acylation, the reaction concentration is low, the cycle is long and the conversion rate is not high, the general sucrose-6-ester product yield is 65-75%, and there are many impurities , not easy to purify

Method used

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  • Synthetic method for sucralose
  • Synthetic method for sucralose
  • Synthetic method for sucralose

Examples

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example 1

[0013] Example 1: Add 100g of sucrose to 300ml of N,N-dimethylformamide, heat to 80°C to dissolve, cool down to 60°C, then add 75g of dibutyltin oxide and stir, add 250ml of cyclohexane to reflux for dehydration reaction, When the dehydration amount reaches 30ml, lower the temperature to -5°C, start to add 40g of acetic anhydride dropwise, and finish the drop within 20 minutes. Organotin was extracted four times, 300ml each time, and the first cyclohexane extract was used to recover organotin, and the 2, 3, and 4 times were applied in sequence; after separating the cyclohexane layer, a light red sucrose-containing 6-ester N,N-dimethylformamide solution, and then add 250ml of cyclohexane to the solution, reflux dehydration at 85-90°C, when the dehydration amount reaches 45-55ml, cool down to stop the reflux, and drop to room temperature Finally, use a separatory funnel to divide the cyclohexane layer to obtain 320ml of anhydrous sucrose-6-ester solution. Our acylation reaction ...

example 2

[0014] Example 2: Heat 100g of sucrose to 85°C and dissolve it in 500ml of N,N-dimethylformamide, then cool down to 65°C, then add 90g of dibutyltin oxide and stir, add 500ml of cyclohexane to reflux for dehydration, when When the amount of dehydration reaches 35ml, cool down to 0°C, start to add 60g of acetic anhydride dropwise, usually within 50 minutes, then keep it at 0°C for 30 minutes, add 10ml of water to stop the reaction, then take cyclohexane and divide it into four Extract the organotin twice, 300ml each time, and separate the cyclohexane layer to obtain a light red N,N-dimethylformamide solution containing sucrose-6-ester, and then add 250ml of cyclohexane to the solution , when the dehydration amount reaches 45-55ml, cool down and stop reflux, and then use a separatory funnel to separate the cyclohexane layer after cooling down to room temperature to obtain 510ml of anhydrous sucrose-6-ester solution for the next step of chlorination; first prepare vissmer Reagent...

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Abstract

The invention belongs to the field of a synthetic method and especially relates to the field of the synthetic method for a sucralose. The synthetic method for the sucralose is characterized in that the method comprises an esterification reaction, a chlorination reaction and a deacetylation reaction of sucralose-6-acetate. The method of the invention successively solves a problem of 6-hydroxy-group protection, that is to say, dibutyltin oxide is utilized to selectively protect other functional groups near the 6-hydroxy-group and the dibutyltin oxide is retrieved after the 6-hydroxy-group is esterified. The method is ingenious and allows little loss of the dibutyltin oxide during recovery, thereby greatly reducing cost. A domestic leading technology of trans-esterification is adopted for final removal of 6-ester. Crystallization is mild, color of finished products is as white as snow, purity of the products is usually more than 99% and yield is 35 to 40%.

Description

technical field [0001] The invention belongs to the field of synthesis methods, in particular to the field of synthesis methods of sucralose. Background technique [0002] The chemical name of sucralose is: 4.1'.6'-trichloro-4.1'.6'-trideoxygalactosucrose. The early synthesis basically used the whole group protection method. The general practice is to first convert the 4, 1', 6' positions of sucrose into benzoate, and then protect all other hydroxyl groups, and then convert 4, 1', 6' The ester is removed, the chlorine is substituted, and finally the other 5 hydroxyl groups are removed. Although this method can obtain sucralose, the yield is very low, generally around 17%, and expensive reagents such as triphenylphosphine and sodium methylate are used, and the cost is very high and is not suitable for industrial production. The more popular method in recent years is to use the semi-group protection method, that is, first protect the 6-position hydroxyl group, then apply chl...

Claims

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Application Information

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IPC IPC(8): C07H5/02C07H1/00
Inventor 李罡
Owner 李罡
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