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Diminazene aceturate production method

A production method and a triazamidine technology are applied in the field of broad-spectrum anti-blood protozoal drug manufacturing and production, which can solve the problems of unfavorable industrialized production, high synthesis temperature, high methanol volatilization and the like, so as to save reaction time, avoid high temperature reaction, and reduce volatilization Effect

Inactive Publication Date: 2015-05-13
HENAN LINGXIAN SCI & TECHN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a kind of production method of triazine amidine, to overcome the defects of the production method of the prior art that the synthesis temperature is high, the time is long, the process is complicated, the methanol volatilizes a lot, and it is unfavorable for industrialized production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) Preparation of p-nitrobenzonitrile:

[0039] A, make solvent dissolving p-nitrobenzamide with toluene, make p-nitrobenzamide solution; The parts by weight of p-nitrobenzamide are 70, and the parts by weight of toluene are 800;

[0040] B, the p-nitrobenzamide solution is dropped into the reaction kettle, add triethylamine and thionyl chloride to react, set the reaction temperature to be 100°C, and the reaction time is 10h; the parts by weight of triethylamine are 4; chlorine The parts by weight of sulfoxide is 95;

[0041] C, cool down to 20°C, add 500 parts by weight of water and stir for 20 minutes to dilute, add a concentration of 30% sodium hydroxide solution to neutralize to a pH value of 7, filter and put it into a separatory kettle to separate the water. The temperature of the toluene layer was raised to 110°C to distill the toluene out, and the toluene was distilled out in a filter rejection machine, and then dried at 60°C to obtain a p-nitrobenzonitrile fi...

Embodiment 2

[0057] (1) Preparation of p-nitrobenzonitrile:

[0058] A, make solvent dissolving p-nitrobenzamide with toluene, make p-nitrobenzamide solution; The parts by weight of p-nitrobenzamide are 80, and the parts by weight of toluene are 900;

[0059] B, p-nitrobenzamide solution is dropped into the reaction kettle, add triethylamine and thionyl chloride to react, set the reaction temperature to be 110°C, and the reaction time is 12h; the parts by weight of triethylamine are 5; chlorine The parts by weight of sulfoxide is 100;

[0060] C, cool down to 30°C, add 620 parts by weight of water and stir for 30 minutes to dilute, add a concentration of 30% sodium hydroxide solution to neutralize to a pH value of 7, filter and put it into a separatory kettle to separate the water. The temperature of the toluene layer was raised to 110°C to distill the toluene out, and the toluene was distilled out in a filter rejection machine, and then dried at 60°C to obtain a p-nitrobenzonitrile filte...

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Abstract

The invention discloses a diminazene aceturate production method. The method comprises the following steps: reacting p-nitrobenzamide with triethylamine and thionyl chloride to synthesize p-nitrobenzonitrile, and carrying out addition, amination, reduction, diazotization, coupling and salt formation on p-nitrobenzonitrile to obtain diminazene aceturate. P-nitrobenzamide is adopted as a raw material to synthesizes p-nitrobenzonitrile, so high temperature reaction is avoided, and industrial production is facilitated; the addition of urea in the diazotization and coupling reactions is in favor of improving the yield; a reaction product obtained after the coupling reaction undergoes water supply and direct pH adjustment without filtering, heating, dissolving or cooling steps, so the reaction steps are simplified, and the reaction time is shortened; and water and methanol are used as solvents in the salt formation, so the volatilization of methanol is reduced, and the crystal form of diminazene aceturate is obviously improved.

Description

technical field [0001] The invention relates to the technical field of production of broad-spectrum antiblood protozoal drugs, in particular to a production method of triazamidine. Background technique [0002] Triazamidine is a traditionally used broad-spectrum anti-blood protozoal drug, and its Chinese names are also called Benier, Xuechongjing, and Diamidinazine. The cas number is 908~54~3. Its production process is rarely reported, and it is only introduced in the 1980 edition of "National Compilation of Raw Materials Process". [0003] Its specific production method is: use p-nitrobenzoic acid as raw material, cyanide reaction with p-toluenesulfonamide at high temperature to generate p-nitrobenzonitrile (C7H4N202[619~72~7]. Then p-nitrobenzene Nitrile addition, amination, reduction, diazotization, coupling, and salt formation to obtain triazine amidine. ((1), addition, amination, add p-nitrobenzonitrile, methanol, and sodium methoxide to the reaction pot, stir Dissol...

Claims

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Application Information

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IPC IPC(8): C07C257/18
Inventor 郭有钢贺国超刘裕东刘占领
Owner HENAN LINGXIAN SCI & TECHN PHARMA
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