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Synthesizing method of 3,4-dimethylpyrazole phosphate (DMPP)

A technology of dimethylpyrazole phosphate and dimethylpyrazole is applied in the field of synthesis of 3,4-dimethylpyrazole phosphate, and can solve the problem of high price of starting materials, many by-products, and high yield. Low problems, to achieve the effect of cheap raw materials, less environmental pollution and high yield

Active Publication Date: 2014-12-31
SHANGYU SUNFIT CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to overcome the defects of high price of starting raw materials, many by-products and low yield in the synthesis method of 3,4-dimethylpyrazole phosphate so far, aiming to provide a new method for preparing 3 , 4-Dimethylpyrazole Phosphate Method

Method used

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  • Synthesizing method of 3,4-dimethylpyrazole phosphate (DMPP)

Examples

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Embodiment 1

[0022] Add 144g (2.0mol) butanone, 90g (3.0mol) paraformaldehyde, and 5g methanol to the reaction flask, heat up to 40-50°C, add 3g, 10% potassium hydroxide solution dropwise, after the dropwise addition is completed, keep the same temperature After reacting for 15 hours, add 145g (2.3mol) hydrazine hydrate, 200g toluene, 0.5g p-toluenesulfonic acid, heat up and reflux for dehydration reaction, separate the generated water during the reaction until no water is generated, react for 10 hours, and then Add this reaction solution to 1120g, 70% (8.0mol) sulfuric acid solution containing 2g sodium iodide and 0.1g tetrabutylammonium bromide, raise the temperature to 80-90°C and react for 12h, the gas phase detection reaction is complete, and cool down to 30 ℃, use 30% sodium hydroxide solution to adjust the pH to 9, add 200g toluene, separate layers, take the organic phase, and distill off the solvent to obtain 3,4-dimethylpyrazole, 3,4-dimethylpyrazole Dissolve it in 500g of ethanol...

Embodiment 2

[0024] Add 144g (2.0mol) butanone, 90g (3.0mol) paraformaldehyde, and 5g methanol to the reaction flask, heat up to 40-50°C, add 3g, 10% sodium hydroxide solution dropwise, after the dropwise addition, keep the same temperature After reacting for 15 hours, add 145g (2.3mol) hydrazine hydrate, 200g toluene, 0.5g p-toluenesulfonic acid, heat up and reflux for dehydration reaction, separate the generated water during the reaction until no water is generated, react for 10 hours, and then Add this reaction solution to 1120g, 70% (8.0mol) sulfuric acid solution containing 2g sodium iodide and 0.1g tetrabutylammonium bromide, raise the temperature to 70-80°C and react for 14h, the gas phase detection reaction is complete, and cool down to 30 ℃, use 30% sodium hydroxide solution to adjust the pH to 9, add 200g toluene, separate layers, take the organic phase, and distill off the solvent to obtain 3,4-dimethylpyrazole, 3,4-dimethylpyrazole Dissolve it in 500g of ethanol, add phosphoric...

Embodiment 3

[0026]Add 144g (2.0mol) butanone, 90g (3.0mol) paraformaldehyde, and 5g methanol to the reaction flask, heat up to 40-50°C, add 3g, 10% potassium hydroxide solution dropwise, after the dropwise addition is completed, keep the same temperature After reacting for 15 hours, add 145g (2.3mol) hydrazine hydrate, 200g toluene, 0.5g p-toluenesulfonic acid, heat up and reflux for dehydration reaction, separate the generated water during the reaction until no water is generated, react for 10 hours, and then Add this reaction solution to 1120g, 70% (8.0mol) sulfuric acid solution containing 2g sodium iodide and 0.1g tetrabutylammonium bromide, raise the temperature to 80-90°C and react for 12h, the gas phase detection reaction is complete, and cool down to 30 ℃, use 30% sodium hydroxide solution to adjust the pH to 9, add 200g toluene, separate layers, take the organic phase, and distill off the solvent to obtain 3,4-dimethylpyrazole, 3,4-dimethylpyrazole Dissolve in 500g of methanol, a...

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Abstract

The invention discloses a synthesizing method of 3,4-dimethylpyrazole phosphate (DMPP); the method comprises the following steps of taking butanone and paraformal-dehyde as raw materials, and performing four reactions of condensation, cyclization, dehydrogenation and salt-forming to prepare 3,4-dimethylpyrazole phosphate. The raw materials adopted by the invention are low in cost and easy to get, the reaction condition of each step is moderate, the operation is simple, the requirement to equipment is low, the pollution to the environment is less, the yield is high and the purity is good.

Description

(1) Technical field [0001] The present invention relates to a preparation method of 3,4-dimethylpyrazole phosphate (DMPP), in particular to the preparation of 3,4-dimethylpyrazole phosphate by using butanone, paraformaldehyde, hydrazine hydrate and other raw materials Synthetic method, compared with the traditional process, this process is more suitable for industrial production. (2) Background technology [0002] Pyrazole compounds are a class of substances with various biological activities such as antibacterial, antispasmodic, anti-inflammatory, regulating plant growth, and anti-platelet aggregation. They play an important role in medicine and pesticides and are widely used in weeding, insecticide, and fungicide , acaricides and other plant protection agents, as well as heat and light sensitive recording materials. Among the applications of many pyrazole compounds, slow-release fertilizers formed by pyrazole compounds as nitrification inhibitors of nitrogen fertilizers h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D231/12
Inventor 黄生建张春雷徐灿闯
Owner SHANGYU SUNFIT CHEM
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