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Preparation method of sucrose-6-benzoate

A technology of benzoate and methyl benzoate, which is applied in the field of preparation of intermediates, can solve the problems of high toxicity and difficulty in recycling, and achieve the effect of high economy and low requirements for reaction equipment

Active Publication Date: 2012-11-28
天津北方食品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this type of reaction, a large amount of organotin is used as a catalyst for hydroxyl activation, which is highly toxic and difficult to recycle.

Method used

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  • Preparation method of sucrose-6-benzoate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A kind of preparation method of sucrose-6-benzoate, concrete steps are:

[0027] (1) Add 5g of sucrose into a 100ml three-necked round-bottomed flask at a heating temperature of 75°C, dissolve the sucrose in DMF (N,N-dimethylformamide), cool down to room temperature, and obtain a sucrose solution for use , the mass ratio of sucrose to DMF is 1:5 (ie DMF 25g);

[0028] (2) In the reactive distillation device, add cesium carbonate and methyl benzoate to the sucrose solution obtained in step (1), adjust the vacuum degree to 0.05MPa, maintain 55°C, and react for 5h. The amount of cesium carbonate used is sucrose 1% of the mass (i.e. cesium carbonate 0.05g), the molar ratio of sucrose to methyl benzoate is 1:3 (i.e. methyl benzoate 6ml);

[0029] (3) Cool the reaction solution in step (2) to room temperature, add 50ml of dichloromethane to precipitate unreacted sucrose, filter, recover unreacted sucrose, evaporate the solvent in the filtrate under reduced pressure, and obta...

Embodiment 2

[0031] A kind of preparation method of sucrose-6-benzoate, concrete steps are:

[0032] (1) Add 5g of sucrose to a 250ml three-necked round-bottomed flask at a heating temperature of 120°C, dissolve the sucrose in DMSO, cool down to room temperature, and obtain a sucrose solution for use. The mass ratio of sucrose to DMSO is 1 :3;

[0033] (2) In the reactive distillation device, add rubidium carbonate and methyl benzoate to the sucrose solution obtained in step (1), adjust the vacuum degree to 0.05MPa, maintain 60°C, and react for 4 hours. The amount of rubidium carbonate used is sucrose 0.05% of mass, the mol ratio of described sucrose and methyl benzoate is 1:1;

[0034] (3) Cool the reaction solution in step (2) to room temperature, add 50ml of chloroform to precipitate unreacted sucrose, filter, recover unreacted sucrose, and distill off the solvent in the filtrate under reduced pressure to obtain sucrose-6-benzoic acid The ester crude product is 3.6g, the yield is 72%....

Embodiment 3

[0036] A kind of preparation method of sucrose-6-benzoate, concrete steps are:

[0037](1) Add 5g of sucrose to a 100ml three-necked round-bottomed flask at a heating temperature of 40°C, dissolve the sucrose in DMF, cool down to room temperature, and obtain a sucrose solution for use. The mass ratio of sucrose to DMF is 1 :4;

[0038] (2) In the reactive distillation device, add sodium carbonate and methyl benzoate to the sucrose solution obtained in step (1), adjust the vacuum degree to 0.05MPa, maintain 50°C, and react for 5h. The amount of sodium carbonate used is sucrose 2% of mass, the mol ratio of described sucrose and methyl benzoate is 1:2;

[0039] (3) Cool the reaction solution in step (2) to room temperature, add 50ml of 1,2-dichloroethane to precipitate unreacted sucrose, filter to recover unreacted sucrose, evaporate the solvent in the filtrate under reduced pressure, and obtain The crude product of sucrose-6-benzoate was 3.8g, and the yield was 76%. The crude ...

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Abstract

The invention provides a preparation method of sucrose-6-benzoate, which comprises the following steps: by using sucrose as a raw material, methyl benzoate as an esterifying reagent and an alkali carbonate as a catalyst, synthesizing sucrose-6-benzoate under vacuum distillation conditions; and by using the polar difference between the sucrose and the sucrose-6-benzoate, adding a low-polarity solvent to precipitate unreacted sucrose, thereby purifying the sucrose-6-benzoate. The method can enhance the yield and purity of the sucrose-6-benzoate and recycle the unreacted sucrose, has the advantages of environment-friendly technique, low facility request and high economical efficiency, provides a new way for synthesizing sucrose-6-benzoate, and is suitable for the demands for large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of a sucralose intermediate, in particular to a preparation method of sucrose-6-benzoate. Background technique [0002] Sucralose, the English name is Sucralose, is the only functional sweetener that uses sucrose as a raw material, and its sweetness can reach more than 600 times that of sucrose. It is one of the best functional sweeteners currently. [0003] Sucralose is a non-hygroscopic white crystalline powder with high chemical stability in acidic solution and good stability under light and heat conditions. It is easily soluble in ethanol and has a good linear relationship between the refractive index and solubility. [0004] At present, the "single group protection method" is usually used to finally synthesize sucralose. The advantage of this method is that sucralose can be synthesized in three steps by the single-group protection method, with few steps, simple operation, and low requirements on proc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H13/08C07H1/00
Inventor 齐欣李胜彬李娟耿蔚华唐向阳曹世嘉赵温涛常虹
Owner 天津北方食品有限公司
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