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Continuous preparation method of 2-aminomalonamide

A technology of aminomalonamide and diethyl aminomalonate is applied in the field of continuous preparation of 2-aminomalonamide to achieve the effects of improving reaction efficiency, simple amplification and speeding up reaction rate

Pending Publication Date: 2021-09-24
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation methods reported so far are batch reaction methods, and no continuous preparation methods have been reported.

Method used

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  • Continuous preparation method of 2-aminomalonamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Mix diethyl 2-aminomalonate and methanol at a volume ratio of 1:4, then use a high-pressure plunger pump to pump the mixed solution and 25% ammonia water into the pre-mixer at a flow rate ratio of 1:2, and preheat The pipeline is preheated to 45°C, and then enters the microreactor for reaction. The reaction pressure is 2.5Mpa, the reaction temperature is 45°C, and the residence time of the reaction liquid is 11 minutes to obtain a mixed liquid containing 2-aminomalonamide. The mixed liquid is concentrated under reduced pressure to obtain The crude 2-aminomalonamide was purified by beating with methanol, filtered with suction, and the filter cake was air-dried at room temperature to obtain a white or light yellow powdery solid; the yield was 89%. The filtrate evaporates methanol and can be used repeatedly.

Embodiment 2

[0027] This example is the same as Example 1, and the difference with Example 1 is that the reaction temperature in this example is 65°C. The yield thereof was 88.9%.

Embodiment 3

[0029] This example is the same as Example 1, and the difference with Example 1 is that in this example, the reaction temperature is 85° C., and the yield is 84%.

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PUM

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Abstract

The invention discloses a continuous preparation method of 2-aminomalonamide, and belongs to the field of organic synthesis. The method comprises the steps of by taking diethyl 2-aminomalonate as a raw material and ammonia water as an ammonolysis reagent, reacting through a micro-channel reactor at a certain temperature and pressure, and carrying out vacuum concentration to obtain 2-aminomalonamide. The invention provides a continuous preparation process method of 2-aminomalonamide. The method is simple, continuous production can be realized, the reaction time is short, the product yield reaches 80-90%, and the productivity is improved.

Description

technical field [0001] The invention relates to a continuous preparation method of 2-aminomalonamide, which belongs to the technical field of organic synthesis. Background technique [0002] 2-Aminomalonamide is an important chemical synthesis intermediate, widely used in medicine, fertilizer, food and other fields. [0003] Existing many patents have reported the synthetic method of 2-aminomalonamide at present. Publication No. CN110446709A mixed diethyl 2-aminomalonate and ammonia methanol, stirred overnight at 80°C under airtight conditions, concentrated under reduced pressure, and reported a yield of 73%. Publication number CN108250104 adopts NH 4 Aqueous Cl solution was used as ammonium solution reagent, and the reaction was refluxed at 100°C for two hours, with a reported yield of 87%. Although the yield of this method is not low, it is difficult to deal with the three wastes and is not suitable for industrialization. Publication No. JP2010241805 uses ammonia water...

Claims

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Application Information

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IPC IPC(8): C07C231/02C07C237/06
CPCC07C231/02C07C237/06
Inventor 高岩汪涛
Owner DALIAN UNIV OF TECH
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