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Prepn process of 2-nitro imido imidazolyl alkane

A technology of nitroiminoimidazolidine and nitroguanidine, which is applied in the field of preparation of 2-nitroiminoimidazolidine, can solve the problem of low yield of 2-nitroiminoimidazolidine, low yield, potassium hydroxide Problems such as high cost of raw materials, to achieve the effect of good product quality, high reaction yield, and low cost of raw materials

Inactive Publication Date: 2007-11-07
NANTONG TENDENCI CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Domestically, there are bibliographical reports (2-nitroimino imidazolidine synthesis new process, Hebei Chemical Industry, 2002 (6), 40) prepared by reacting ethylenediamine dihydrochloride with nitroguanidine. The disadvantage of this method is the use of ethylenediamine Preparation of Compound III, 2-Nitroiminoimidazolidine, by Reaction of Amine Dihydrochloride and Nitroguanidine with Low Yield
[0005] Another bibliographical report (the synthesis of novel insecticide substitution-2-nitroimino-imidazolidine and preliminary efficacy test, Pesticides, 2000 (1), 16-17) nitroguanidine and ethylenediamine hydrochloride in Reaction in potassium hydroxide aqueous solution, the shortcoming of this method is that the raw material cost of potassium hydroxide used is higher, and yield is low

Method used

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  • Prepn process of 2-nitro imido imidazolyl alkane
  • Prepn process of 2-nitro imido imidazolyl alkane

Examples

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Effect test

Embodiment 1

[0018] Pump 150Kg ethylenediamine and 300Kg water into a 1000L reactor, add concentrated sulfuric acid dropwise to neutrality under freezing, put in 260Kg nitroguanidine, stir evenly, add 30% liquid caustic soda dropwise until the pH is 9, heat up to 60°C, and react After 6 hours, cool to room temperature, shake and filter to obtain a wet product, and dry to obtain a 254Kg finished product (above the content of 99%).

Embodiment 2

[0020] Pump 150Kg ethylenediamine and 300Kg water into a 1000L reactor, add concentrated sulfuric acid dropwise to neutrality under freezing, put in 260Kg nitroguanidine, stir well, add 30% liquid caustic soda dropwise until the pH is 10, heat up to 45°C, and react After 2 hours, cool to room temperature, shake and filter to obtain a wet product, and dry to obtain a 243Kg finished product (more than 99% content).

Embodiment 3

[0022] Pump 150Kg ethylenediamine and 300Kg water into a 1000L reactor, add concentrated sulfuric acid dropwise to neutrality under freezing, put in 260Kg nitroguanidine, stir evenly, add 30% liquid caustic soda dropwise until the pH is 8, heat up to 80°C, and react After 10 hours, cool to room temperature, shake and filter to obtain a wet product, and dry to obtain a 230Kg finished product (more than 99% content).

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Abstract

The preparation process of 2-nitro imido imidazolyl alkane belongs to the field of farm chemical intermediate preparing technology. It includes the first reaction between acid and ethylene diamine to obtain ethylene diamine salt, the subsequent reaction between ethylene diamine salt and nitroguanidine, and final filtering and stoving to obtain the 2-nitro imido imidazolyl alkane product. The present invention has the advantages of low material cost, high reaction yield up to 80 % and high product quality, and the product has smelting point of 232-234 deg.c and 2-nitro imido imidazolyl alkane content over 99 %, and is white or yellowish crystal.

Description

technical field [0001] The invention relates to a preparation method of 2-nitroiminoimidazolidine, belonging to the technical field of pesticide intermediates. Background technique [0002] 2-Nitroiminoimidazolidine is an important pesticide intermediate and an important raw material for imidacloprid. Its structural formula is as follows: [0003] [0004] There are literature reports in China (2-nitroiminoimidazolidine synthesis new process, Hebei Chemical Industry, 2002 (6), 40) prepared by the reaction of ethylenediamine dihydrochloride and nitroguanidine. The shortcoming of this method is to use ethylenediamine The yield of compound III, 2-nitroiminoimidazolidine, was prepared by reacting amine dihydrochloride with nitroguanidine. [0005] Another bibliographical report (the synthesis of novel insecticide substitution-2-nitroimino-imidazolidine and preliminary efficacy test, Pesticides, 2000 (1), 16-17) nitroguanidine and ethylenediamine hydrochloride in Reaction i...

Claims

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Application Information

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IPC IPC(8): C07D233/52
Inventor 查志明吕国华
Owner NANTONG TENDENCI CHEM
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