Method for preparing neotame

A neotame and solvent technology, applied in the field of chemistry, can solve problems such as unfavorable industrialized production, complex process operation, low yield and the like, and achieve the effects of being beneficial to environmental protection, reducing environmental pollution and high economic benefits

Inactive Publication Date: 2011-08-31
宁宗超
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The preparation method uses a metal catalyst, which has high cost, complex process operation, and requires a hydrogen source
[0010] Provided in U.S. Patent No. 5,480,668 is a method for preparing neotame by reducing the reactant of aspartame and 3,3-dimethylbutyraldehyde with sodium cyanoborohydride as a reducing agent. Due to the price of sodium cyanoborohydride It is more expensive, and there is a danger of producing cyanide when the acidity in the reaction is strong, which is not conducive to industrial production
[0011] Chinese patent CN101270092A provides a method for preparing neotame by reducing the reactant of aspartame and 3,3-dimethylbutyraldehyde with formic acid as a reducing agent. The reaction of this preparation method is incomplete and the yield is low (about 60%)

Method used

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  • Method for preparing neotame
  • Method for preparing neotame

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment one kind of preparation method of neotame, contains following preparation steps:

[0031] (1). Add 10g of aspartame to 100ml of methanol, add 3,3-dimethylbutyraldehyde, and react at a temperature of 50°C for 3 hours;

[0032] (2). Add sodium acetate borohydride to the above reaction solution, and react at a temperature of 50°C for 2 hours;

[0033] (3). The above reaction solution was extracted with water and ethyl acetate at a volume ratio of 4:6, and the organic layer was dried;

[0034] (4). The dried product obtained above was crystallized with water and ethanol at a volume ratio of 3:7 to obtain 11.3 g of neotame.

[0035] In this example, neotame yield was 88%.

[0036] The neotame prepared in this example has a purity of 98.9% as measured by high performance liquid chromatography (HPLC) according to the US Pharmacopoeia 33rd edition.

Embodiment 2

[0037] Embodiment two a kind of preparation method of neotame, contains following preparation steps:

[0038] (1). Add 15g of aspartame to 100ml of tetrahydrofuran, add 3,3-dimethylbutyraldehyde, and react at 30°C for 2 hours;

[0039] (2). Add sodium acetate borohydride to the above reaction solution, and react at a temperature of 30°C for 3 hours;

[0040] (3). The above reaction solution was extracted with water and dichloromethane at a volume ratio of 5:5, and the organic layer was dried;

[0041] (4). The dried product obtained above was crystallized with water and acetone at a volume ratio of 5:5 to obtain 17.2 g of neotame.

[0042] In this example, the yield of neotame was 89%, and the purity by HPLC was 98.5%.

Embodiment 3

[0043] Embodiment three a kind of preparation method of neotame, contains following preparation steps:

[0044] (1). Add 12g of aspartame to 100ml of tetrahydrofuran, add 3,3-dimethylbutyraldehyde, and react at 60°C for 2 hours;

[0045] (2). Add sodium acetate borohydride to the above reaction solution, and react at 60°C for 1 hour;

[0046] (3). The above reaction solution was extracted with water and dichloromethane at a volume ratio of 5:5, and the organic layer was dried;

[0047] (4). The dried product obtained above was crystallized with water and acetone at a volume ratio of 4:6 to obtain 13.4 g of neotame.

[0048] In this example, the yield of neotame was 87%, and the purity by HPLC was 99.1%.

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Abstract

The invention belongs to chemical sciences, and in particular discloses a method for preparing neotame. The method comprises the following steps of: reducing reactants of aspartame and 3,3-dimethyl butyraldehyde to prepare neotame by taking sodium triacetoxyborohydride as a reducing agent; and reducing a reaction solution of the aspartame and the 3,3-dimethyl butyraldehyde, extracting and crystallizing to obtain the neotame. The method for preparing the neotame is easy and convenient to operate, environmental pollution is reduced, and an obtained product has high purity and high yield.

Description

technical field [0001] The invention relates to the technical field of chemistry, in particular to a method for preparing sweetener neotame. Background technique [0002] Neotame chemical name N-[N-(3,3-dimethylbutyl)-L-a-asparagine]-L-phenylalanine-1-methyl ester, white crystalline powder, specific optical rotation The temperature is -40.0~-43.4 (5mg / ml, water), and its structural formula is as follows (I): [0003] [0004] On July 9, 2002, the US Food and Drug Administration (FDA) officially approved neotame as a sweetener and flavor enhancer for general use in various foods and beverages. On March 10, 2003, the Ministry of Health of China approved neotame as a sweetener for general use in various foods and beverages, and the amount of use depends on production needs. This sweetener is the only sweetener in China's "Hygienic Standards for Food Additives" that has no limit on the scope of use and no limit on the amount of use. [0005] Neotame is about 10,000 times s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K1/00C07K5/072
Inventor 宁宗超唐帅白水昭
Owner 宁宗超
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