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Synthesis process of acesulfame potassium

A technology for the synthesis of acesulfame potassium and its synthesis technology, which is applied in the field of synthesis of acesulfame potassium, and can solve problems such as high cost, low yield of AK sugar, and reduced product quality, and achieve good product quality, simple process, and low cost Effect

Inactive Publication Date: 2010-07-28
GUANGDONG FOOD IND INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Due to the high cost of sulfamic acid fluoride, process 1 has no cost advantage compared with process 2; now, many domestic and foreign manufacturers of AK sugar use process 2 as the production process, but diketene has high activity to form acetoacetamidosulfonic acid tris There are more by-products to generate in the reaction of ethylamine salt, and the yield of triethylamine salt of acetoacetamidosulfonic acid is unsatisfactory, cause the yield of final AK sugar to be lower, in addition, there will be organic impurity 5 in the reaction -Chloro-AK sugar is formed, which is difficult to remove and reduces the quality of the product
[0008] In the process of developing the synthesis process of acesulfame potassium, researchers once wanted to use acetoacetamide as a raw material to synthesize and produce AK sugar. However, due to the limitation of the development level of the acetic acid industry at that time, acetoacetamide could not be produced on a large scale and used in the chemical industry. unrealized

Method used

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  • Synthesis process of acesulfame potassium

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Take 5.0 g (50 mmol) of acetoacetamide, add 50 ml of chloroform and 50 mg of 4-N, N-dimethylaminopyridine (DMAP), stir vigorously, cool down with an ice-salt bath, and control the temperature at -30 to -25 ° C, slowly Add a solution of 10ml of chlorosulfonic acid and 10ml of chloroform, keep stirring at low temperature for 1.0 hours after the addition, raise the temperature to -10°C, slowly add 8ml of water, then stir for 45 minutes, let stand to separate layers, add 20ml to the water layer Extract with chloroform, remove the water phase, combine the organic phases and add 50ml of water, neutralize with 10% potassium hydroxide to pH=7.5, let stand to separate layers, recover the solvent chloroform, spin dry the water under reduced pressure to obtain the crude product of acesulfame potassium 7.2 g was dissolved in an appropriate amount of water and heated to a slight boil, 50 mg of activated carbon was added to reflux for 10 minutes, and 6.5 g of the product was obtained ...

Embodiment 2

[0027] Take 5.0g (50mmol) of acetoacetamide, add 50ml of dichloromethane and 50mg of 4-N,N-dimethylaminopyridine (DMAP), stir vigorously, cool down with an ice-salt bath, and control the temperature at -30~-25°C , slowly add a solution of 10ml of chlorosulfonic acid and 10ml of dichloromethane, keep stirring at low temperature for 1.0 hour after the addition, raise the temperature to -10°C and slowly add 8ml of water, then stir for 45 minutes, let stand to separate layers, and Add 20ml of chloroform to the aqueous layer for extraction, remove the aqueous phase, combine the organic phases and add 50ml of water, neutralize with 10% potassium hydroxide to pH = 7.5, let stand to separate layers, recover the solvent chloroform, spin dry under reduced pressure to obtain crude acetyl 7.3 g of crude potassium sulfamate was dissolved in an appropriate amount of water and heated to a slight boil, 50 mg of activated carbon was added to reflux for 10 minutes, and 6.6 g of the product was o...

Embodiment 3

[0029] Take 5.0g (50mmol) of acetoacetamide, add 50ml of dichloroethane and 50mg of 4-N,N-dimethylaminopyridine (DMAP) and stir vigorously, cool down with an ice-salt bath, and control the temperature at -30~-25°C , slowly add a solution of 10ml of chlorosulfonic acid and 10ml of dichloroethane, keep stirring at low temperature for 1.0 hour after the addition is complete, raise the temperature to -10°C, slowly add 8ml of water, then stir for 45 minutes, let stand to separate layers, Add 20ml of chloroform to the aqueous layer for extraction, remove the aqueous phase, combine the organic phases and add 50ml of water, neutralize with 10% potassium hydroxide to pH = 7.5, let stand to separate layers, recover the solvent chloroform, spin dry the water under reduced pressure to obtain the crude product 7.2 g of crude acesulfame potassium was dissolved in an appropriate amount of water and heated to a slight boil, 50 mg of activated carbon was added to reflux for 10 minutes, and 6.5 ...

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Abstract

The invention discloses a synthesis process of acesulfame potassium, which uses acetylacetamide as raw material and inert organic solvent as solvent. Under the low temperature of -50-15 DEG C, catalyst and cyclizing reagent are added for ring closure reaction, after the reaction, the temperature is controlled in the range of -15-60 DEG C, and water is added for hydrolysis; after the hydrolysis, the reaction liquid stands to laminate, the water layer is extracted by the inert organic solvent to remove the aqueous phase and combine the organic phase, then water is added in the organic phase to wash and remove the aqueous phase, base is added in the organic phase for neutralizing and resting to laminate, the organic phase is recycled and the aqueous phase is decompressed and concentrated to obtain the crude acesulfame potassium, and finally the pure acesulfame potassium is obtained through decoloration by activated carbon and purification by recrystallization. The synthesis process of the acesulfame potassium uses the acetylacetamide as the raw material and has the characteristics of simple process, short procedure, low cost and good product quality.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a synthesis process of acesulfame potassium. Background technique [0002] The chemical name of acesulfame potassium is: 6-methyl-1,2,3-oxazin-4-(3H)-one-2,2-potassium dioxide, and the English name is: 3,4-Dihydro- 6-methyl-1,2,3-oxathiazin-4-one 2,2-dioxide potassium salt. Its structural formula is: [0003] [0004] Acesulfame potassium is a high-intensity sweetener, the chemical name is 6-methyl-1,2,3-oxazin-4-(3H)-one-2,2-dioxyl potassium salt, generally called AK Sugar, commonly known as acesulfame potassium, is the fourth generation of synthetic sweeteners. In 1967, German doctor Karl Clauss found that the product had a sweet taste when he was experimenting with the reaction of butyne and fluorosulfonyl isocyanate. Then he traced the source of the sweetness and finally discovered AK sugar. Now AK sugar has been widely used in food and beverage , healthcare...

Claims

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Application Information

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IPC IPC(8): C07D291/06
Inventor 李家林杜晨光张素娟
Owner GUANGDONG FOOD IND INST
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