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Process for preparing aspartame

A technology of aspartame and aspartic acid, applied in the direction of peptides, etc., can solve the problems of low yield of aspartame products, long reaction cycle, long process, etc., and achieve convenient post-processing and reuse and low processing cost Low, highly selective effect

Inactive Publication Date: 2006-09-13
CHANGZHOU NIUTANG CHEM PLANT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the above-mentioned process route is generally adopted by everyone, there are deficiencies such as many processes, long process, long reaction cycle, and low yield of aspartame products. Other methods of chemically synthesizing aspartame also have similar problems.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A 500ml four-neck round bottom flask with mechanical stirring, thermometer, condenser. Add 160g of 50wt% sodium hydroxide solution into the flask, cool to 0°C, add 133g of L-aspartic acid in batches, and keep the temperature below 0°C. After the addition, 150 g of ethyl thiomethyl formate and 80 g of methanol were added. Slowly raise the temperature to 45°C and stir for 2 hours. After the feed liquid was cooled to room temperature, it was left to stand for 1 hour, and the feed liquid was separated. Cool the water layer to 0°C, slowly add 180ml of concentrated hydrochloric acid with a content of 35wt%, adjust the pH to about 3, add 600ml of ethyl acetate for extraction in 3 times, combine the extracts, wash once with saturated saline, and add the feed solution to 15g of anhydrous magnesium sulfate was dried. Filter and collect the filtrate for concentration. The concentrated solution was filtered again, and the filter cake was dried to obtain 200 g of acylate, with a...

Embodiment 2

[0032] A 500ml four-neck round bottom flask with mechanical stirring, thermometer, condenser. Add 160g of sodium hydroxide solution with a content of 50wt% into the flask, cool to 0°C, add 133g of L-aspartic acid in batches, and keep the temperature below 0°C. After the addition, 150 g of ethyl thiomethyl formate and 80 g of methanol were added. Slowly raise the temperature to 50°C, and stir the reaction for 2 hours. Then, after the feed liquid was cooled to room temperature, it was allowed to stand for 1 hour, and the feed liquid was separated. Then the separated water layer was cooled to 10°C, and 150ml of 35wt% concentrated hydrochloric acid was slowly added to adjust the pH to about 3.5; 600ml of ethyl acetate was added in 3 times for extraction, the combined extracts were washed once with saturated brine . Add 15 g of anhydrous magnesium sulfate to the washed feed liquid to dry, filter, and collect the filtrate for concentration. The concentrate was filtered again, an...

Embodiment 3

[0037] A 500ml four-neck round bottom flask with mechanical stirring, thermometer, condenser. Add 120g of 50wt% sodium hydroxide solution into the flask, cool to 0°C, add 133g of L-aspartic acid in batches, and keep the temperature below 0°C. After the addition, 150 g of ethyl thiomethyl formate and 80 g of methanol were added. Slowly raise the temperature to 45°C and stir for 2 hours. After the feed liquid was cooled to room temperature, it was left to stand for 1 hour, and the feed liquid was separated. Then the separated water layer was cooled to 0°C, and 180ml of concentrated hydrochloric acid with a content of 35wt% was slowly added to adjust the pH to about 3, and 600ml of ethyl acetate was added for extraction in 3 times, the combined extracts were washed once with saturated saline . Add 15g of anhydrous magnesium sulfate to the washed feed liquid to dry. Filter and collect the filtrate for concentration. The concentrated solution was filtered again, and the filter...

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PUM

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Abstract

The invention relates to aspartame preparation by chemical synthesis method. A vulcanizing and acylating agent is used as a protective agent for protection and activation for amino and alpha-carboxyl of L-aspartic acid, and the acylate of the L-aspartic acid is prepared. Then a cyclization reagent is added for cyclization reaction and a cyclics is generated. The aspartame product is obtained from the cyclics by condensation. The aspartame product has less pollution to environment, and has a high purity and a high yield.

Description

technical field [0001] The present invention relates to a preparation method of aspartame, in particular to the preparation of aspartame by chemical synthesis, especially the preparation of aspartame by using L-aspartic acid and L-phenylalanine methyl ester hydrochloride as raw materials The method for bartame belongs to the technical field of chemical synthesis. Background technique [0002] Aspartame (Aspartame, C 14 h 18 N 2 o 5 ), the chemical name is α-L-aspartoyl-L-phenylalanine methyl ester, commonly known as sweetener, which is a new synthetic sweetener. In 1965, the American GDSearle Company synthesized aspartame for the first time and obtained a patent right. Aspartame is a white crystalline powder with a refreshing sweetness, and its sweetness is 180-200 times that of sucrose. Compared with synthetic sweeteners such as saccharin, cyclamate, and AK sugar, it has the advantages of good taste, high safety, and low calorie, making it popular in the European and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07K5/075
Inventor 王方大蔡亚王立成
Owner CHANGZHOU NIUTANG CHEM PLANT CO LTD