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Synthesis method of 3-acetyl-4-nitroimino-1, 3, 5-oxadiazine

The technology of a nitroimino group and a synthesis method is applied in the field of synthesis of 3-acetyl-4-nitroimino-1,3,5-oxadiazine, and can solve the problem of low yield, inability to effectively obtain products, The market development process is hindered and other problems, to achieve the effect of the safety of the preparation method

Pending Publication Date: 2022-06-10
NANTONG TENDENCI CHEM
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Problems solved by technology

However, the corresponding large-scale production process has not yet been formed in the industry. The yield of conventional preparation methods is extremely low, and related products cannot be effectively obtained, which seriously hinders the market development process.

Method used

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  • Synthesis method of 3-acetyl-4-nitroimino-1, 3, 5-oxadiazine

Examples

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Embodiment Construction

[0016] The technical solution of the present invention will be further described below in conjunction with the examples. The technical schemes and related parameters given in the following embodiments are only exemplary, and are intended to explain the present invention, but should not be construed as limiting the present invention.

[0017] This example discloses a synthesis method of 3-acetyl-4-nitroimino-1,3,5-oxadiazine, the specific operation is as follows:

[0018] Add 90g of paraformaldehyde and 300g of 20% formic acid in sequence in a 1000ml four-neck flask, heat up to 50°C for reaction, put in 104g of nitroguanidine after 2 hours, heat up to 70°C for reaction, and keep warm for 10h; after the reaction is completed, add potassium carbonate to neutralize the pH to 7-8, filtered, washed and dried to obtain 4-nitroimino-1,3,5-oxadiazine.

[0019] Add 200g of toluene and 4-nitroimino-1,3,5-oxadiazine into a 1000ml four-necked flask and mix, gradually add 86.5g of acetyl c...

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Abstract

The invention provides a synthesis method of 3-acetyl-4-nitroimino-1, 3, 5-oxadiazine, which comprises the following steps: mixing 20% formic acid with paraformaldehyde, heating to 50 DEG C, preserving heat for 2 hours, adding nitroguanidine, continuously heating to 70 DEG C, preserving heat for 10 hours, and synthesizing an intermediate 4-nitroimino-1, 3, 5-oxadiazine; and dissolving the dried 4-nitroimino-1, 3, 5-oxadiazine in methylbenzene, dropwise adding acetyl chloride, heating to 40 DEG C, reacting for 2-3 hours, cooling and filtering to obtain the 3-acetyl-4-nitroimino-1, 3, 5-oxadiazine. The yield of the prepared product is increased to 85%, and the content of the product is increased to 99%; the preparation method is safe, environment-friendly and suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a synthesis method of 3-acetyl-4-nitroimino-1,3,5-oxadiazine, which belongs to the technical field of organic synthesis. Background technique [0002] 3-Acetyl-4-nitroimino-1,3,5-oxadiazine is a neonicotinoid insecticide intermediate, which is a new type of insecticide with high efficiency, low toxicity, safety and high selectivity Compared with the current commercial neonicotinoid insecticides, it has the advantages of lower application dosage and wider insecticidal spectrum, and has a good application prospect. However, there is no corresponding large-scale production process in the industry at present, and the yield of conventional preparation methods is extremely low, and related products cannot be obtained effectively, which seriously hinders the market development process. Contents of the invention [0003] The purpose of the present invention is to solve the above-mentioned defect that existing acetyl oxadiazine synth...

Claims

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Application Information

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IPC IPC(8): C07D273/04
CPCC07D273/04
Inventor 张赟
Owner NANTONG TENDENCI CHEM