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Preparation method of nicarbazin midbody 4,4'- binitro sym-diphenylurea

A technology of diphenylurea and dinitro, which is applied in the synthesis of intermediates of veterinary drugs, dyes and medicines, and in the field of organic chemical industry. The effect of high efficiency and simple process

Active Publication Date: 2010-12-15
MASTEAM BIO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Obviously, in addition to the use of expensive catalysts, this process is expensive, and the large-scale microwave devices used in industry are currently difficult to obtain.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] p-Nitroaniline (1.3mol), urea (1mol) was added in the reaction flask, then 2mol of concentrated hydrochloric acid (according to the amount of HCl) of 35wt% was added, under stirring, heated at 185°C and the hydrochloric acid was steamed out, After the liquid solidifies (1.5 hours), continue heating at this temperature for 2.5 hours. Add 300mL of DMF, heat to boiling, make the lumpy solid into a small granular solid that can be stirred, and cool to room temperature. Filtration, DMF recovery, for the next processing block solid. The filtered solid was washed twice with water and twice with ethanol, dried and weighed to obtain 172 g of a yellow needle-like solid with a yield of 88%. The melting range of the product is: 315°C to 317°C, and the literature value is: 318°C to 319°C.

Embodiment 2

[0012] P-nitroaniline (1.3mol), urea (0.8mol) was added in the reaction flask, then added 2.5mol of 35wt% concentrated hydrochloric acid (according to the amount of HCl substance), under stirring, heated at 200°C and distilled the hydrochloric acid After the liquid is solidified (about 50 minutes), continue heating at this temperature for 1 hour. Add 400mL of DMF, heat to boiling, make the lumpy solid into a small granular solid that can be stirred, and cool to room temperature. Filtration, DMF recovery, for the next processing block solid. The filtered solid was washed twice with water and twice with ethanol, dried and weighed to obtain 166 g of yellow needle-like solid with a yield of 85%. The melting range of the product is: 315°C to 317°C, and the literature value is: 318°C to 319°C.

[0013] Synthesis of Nicarbazine

[0014] Add 4,4'-dinitrodiphenylurea, urea, absolute ethanol, acetylacetone and concentrated hydrochloric acid into the reaction flask in turn, and reflux...

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Abstract

The invention relates to a preparation method of 4,4'-binitro sym-diphenylurea, comprising the following steps of: adding paranitroaniline, urea and concentrated hydrochloric acid to a reactor, and reacting for 1-5 hours at 180-200 DEG C under stirring, and purifying to obtain the 4,4'-binitro sym-diphenylurea. The invention has simple process, low cost and high yield, does not use an organic solvent in the reaction process and is suitable for industrial production.

Description

technical field [0001] The invention relates to a synthesis method of veterinary drug nicarbazine intermediate 4,4'-dinitrodiphenylurea. The invention belongs to the technical field of organic chemical industry, and also belongs to the technical field of intermediate synthesis of veterinary drugs, dyes and medicines. Background technique [0002] In the production of nicarbazine, the key is the synthesis of 4,4'-dinitrodiphenylurea. Generally, it is prepared by the reaction of phosgene, solid phosgene and urea with p-nitroaniline. The use of phosgene has a high yield but phosgene is highly toxic; the use of solid phosgene can also obtain high yield, but the price of solid phosgene is high, which will increase the cost, and solid phosgene will also produce highly toxic light during use and storage. Gas, there is a safety issue. Using urea as a raw material is cheap and non-toxic, and is an ideal raw material. Therefore, there are many reports on the development of urea as ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C275/30C07C273/18C07D239/36
Inventor 彭要武田文敬朱正宇
Owner MASTEAM BIO TECH
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