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Preparation method of 2-aminomalonamide

A technology of aminomalonamide and diethyl aminomalonate, applied in the field of chemical preparation, can solve the problems of long cycle, low purity and high equipment requirements, and achieve the effects of simple operation, high yield and low cost

Active Publication Date: 2021-12-24
SHANDONG CHENGCHUANG BLUE OCEAN PHARM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the prior art basically adopts 2-aminomalonate diethyl ester or its hydrochloride and ammonia to prepare 2-aminomalonamide; Technical defects such as high equipment requirements (such as requiring equipment to resist corrosion) make the synthesis of 2-aminomalonamide unfavorable for industrialization; it cannot meet production needs

Method used

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  • Preparation method of 2-aminomalonamide
  • Preparation method of 2-aminomalonamide
  • Preparation method of 2-aminomalonamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Pass 24.1g of ammonia gas into 200g of purified water and lower the temperature to 10°C, add dropwise a solution consisting of 100g of diethyl 2-aminomalonate hydrochloride and 100g of purified water, after the addition is complete, at a temperature of 10°C Heat preservation reaction. After the reaction, drop to -8°C to crystallize for 2 hours, filter, and dry at 50°C for 8 hours to obtain 50.89 g of product. During the reaction process, the liquid phase is centrally controlled, and the reaction process is monitored by HPLC method. The monitoring results show that after the dropwise addition, the reaction ends in 6 hours.

[0047] The obtained product is detected by mass spectrometry, and the detection results are as follows: figure 1 As shown, the molecular weight is 118.0588 (the molecular weight detected by positive ion mass spectrometry is 118.0588, and the actual molecular weight is 117.0588), and the charge-to-mass ratio (m / z) is 117.05. according to figure 1 It...

Embodiment 2

[0051] Pass 150.5g of ammonia gas into 1000g of purified water and cool down to 0°C, add dropwise a solution consisting of 500g of diethyl 2-aminomalonate hydrochloride and 500g of purified water, after the addition is completed, the temperature of 0°C Heat preservation reaction. After the reaction, drop to -5°C to crystallize for 2 hours, filter, and dry at 55°C for 8 hours to obtain 257.25 g of product. During the reaction process, the liquid phase is centrally controlled, and the reaction process is monitored by HPLC. The monitoring results show that after the dropwise addition, the reaction ends in 8 hours.

[0052] The obtained product is detected by mass spectrometry, and it can be confirmed that the obtained product is 2-aminomalonamide according to the detection data.

[0053] In terms of 2-aminomalonate diethyl ester hydrochloride, the yield of gained 2-aminomalonamide is 93%, and the prepared 2-aminomalonamide is analyzed by high performance liquid phase, and the detec...

Embodiment 3

[0056] Pass 4.01kg of ammonia gas into 40kg of purified water and lower the temperature to -5°C, add dropwise a solution of 10kg of 2-aminomalonate diethyl hydrochloride and 10kg of purified water, after the dropwise addition, the temperature condition of 5°C The reaction was carried out under heat preservation. After the reaction was completed, the temperature was lowered to -8°C to crystallize for 3 hours, filtered, and dried at 50°C for 8 hours to obtain 5.15 kg of the product. During the reaction process, the liquid phase is centrally controlled, and the reaction process is monitored by HPLC method. The monitoring results show that after the dropwise addition, the reaction ends in 7 hours.

[0057] The obtained product is detected by mass spectrometry, and it can be confirmed that the obtained product is 2-aminomalonamide according to the detection data.

[0058] In terms of 2-aminomalonate diethyl ester hydrochloride, the yield of gained 2-aminomalonamide is 93.1%, and th...

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Abstract

The invention relates to a preparation method of chemicals, in particular to a preparation method of 2-aminomalonamide. The invention provides a synthesis method of 2-aminomalonamide, which comprises the following steps: dropwise adding a solution of diethyl 2-aminomalonate hydrochloride into ammonia water, and controlling the reaction temperature to be below 10 DEG C; and after the reaction is finished, crystallizing to obtain a solid, namely the 2-aminomalonamide. The synthesis method is short in production period and beneficial to reduction of production cost; only two steps of dropwise adding and devitrifying are needed, so that the operation is simple; and only one reaction container is needed in the whole process, and the reaction container does not need to be replaced in the process, so that the production efficiency is improved. The purity of the prepared 2-aminomalonamide is up to 99.5% or above, and the yield of the 2-aminomalonic acid diethyl ester hydrochloride is up to 99.0% or above.

Description

technical field [0001] The invention relates to a preparation method of chemicals, in particular to a preparation method of 2-aminomalonamide. Background technique [0002] 2-aminomalonamide is an important intermediate for the production of 5-hydroxyl-1H-imidazole-4-carboxamide and favipiravir, and its consumption is large, requiring mass production. [0003] At present, the prior art basically adopts 2-aminomalonate diethyl ester or its hydrochloride and ammonia to prepare 2-aminomalonamide; Technical defects such as high equipment requirements (such as requiring equipment to be corrosion-resistant) make the synthesis of 2-aminomalonamide unfavorable for industrialization; it cannot meet production needs. Contents of the invention [0004] The purpose of this application is to provide a kind of synthetic method of 2-amino malonamide. The synthesis method of 2-aminomalonamide provided by the application has high yield, high purity and short production cycle, which is be...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C231/24C07C237/06
CPCC07C231/02C07C231/24C07C237/06
Inventor 王庭见陆红林张风英岳丽丽王荣坤刘凤祥陈文更
Owner SHANDONG CHENGCHUANG BLUE OCEAN PHARM TECH CO LTD
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