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Preparation method of 3, 4-dimethylpyrazole and phosphate thereof

A technology of dimethylpyrazole and dimethylformamide, which is applied in the field of preparation of 3,4-dimethylpyrazole and its phosphate, can solve the problems of complex process, high production difficulty and high cost of raw materials, Achieve the effect of easy availability of raw materials, high product quality and cheap raw materials

Pending Publication Date: 2020-03-10
武威金仓生物科技有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the problems in the existing 3,4-dimethylpyrazole and its phosphate synthesis process, such as complex process, high cost of raw materials, environmental pollution, and high difficulty in industrialized scale-up production, the present invention proposes a 3,4-dimethylpyrazole Preparation method of pyrazole and phosphate thereof

Method used

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  • Preparation method of 3, 4-dimethylpyrazole and phosphate thereof
  • Preparation method of 3, 4-dimethylpyrazole and phosphate thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Preparation of 3,4-dimethylpyrazole phosphate:

[0032] Add 109.5g (1.8eq.) of N,N-dimethylformamide and 350mL of dichloromethane into the reaction flask, and slowly add 229.6g (1.8eq.) of phosphorus oxychloride dropwise under control of the internal temperature at 0-20°C. Stir for 30 minutes; control the internal temperature to 0-20°C, then slowly add 60g (1eq.) 2-butanone dropwise, keep at 0-20°C for 3 hours after the dropwise addition, then raise the temperature to 30-40°C and continue the reaction for 2 hours . After the reaction, cool down to 15-25°C and add water, extract and separate the aqueous phase obtained by dichloromethane and extract once more, combine the organic phases, concentrate under reduced pressure to 120-130mL, and obtain the formylated alkenyl chloride compound of organic solutions.

[0033] Add the organic solution of the above-mentioned formylated alkenyl chloride compound (3-chloro-2-methyl-3-butene-1-aldehyde) into a three-necked flask, slo...

Embodiment 2

[0036] Add 255g (2.9eq.) N,N-dimethylformamide and 400mL 1,2-dichloroethane into the reaction flask, and slowly add 127.7g (1eq.) trichloroxy Phosphorus, stir for 30 minutes; control the internal temperature at 0-20°C and then slowly add 60g (1eq.) 2-butanone dropwise, keep the reaction at 0-20°C for 3 hours after the dropwise addition, then raise the temperature to 30-40°C to continue the reaction 2 hours. After the reaction is over, cool down to 15-25°C and add water, extract and separate the aqueous phase obtained by extracting once more with 1,2-dichloroethane, combine the organic phases, concentrate under reduced pressure to 120-125mL, and obtain the aldehyde group Organic solutions of alkenyl chloride compounds.

[0037] Add the organic solution of the above-mentioned formylated alkenyl chloride compound (3-chloro-2-methyl-3-butene-1-aldehyde) into a three-necked flask, slowly add 52g of 80% hydrazine hydrate solution dropwise, and then control the temperature for 15 Slo...

Embodiment 3

[0040] Add 121.6g (2eq.) of N,N-dimethylformamide and 500mL of methyl tert-butyl ether into the reaction flask, and slowly add 191.4g (1.5eq.) of oxytrichloride dropwise under control of the internal temperature at 0-20°C Phosphorus, stir for 30 minutes; control the internal temperature at 0-20°C and then slowly add 60g (1eq.) 2-butanone dropwise, keep the reaction at 0-20°C for 3 hours after the dropwise addition, then raise the temperature to 30-40°C to continue the reaction 2 hours. After the reaction, the temperature was lowered to 15-25°C and water was added, and the aqueous phase obtained after extraction and separation was extracted once more with methyl tert-butyl ether, and the organic phases were combined and concentrated under reduced pressure to 120-125 mL.

[0041] Add the organic solution of the above-mentioned formylated alkenyl chloride compound (3-chloro-2-methyl-3-butene-1-aldehyde) into a three-necked flask, slowly add 52g of 80% hydrazine hydrate solution d...

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Abstract

The invention relates to a preparation method of 3, 4-dimethylpyrazole and phosphate thereof, and the method of the 3, 4-dimethylpyrazole comprises the following steps: 1) reacting 2-butanone, phosphorus oxychloride and N, N-dimethylformamide in a reaction solvent at -10 to 70 DEG C, and separating and extracting to obtain a solution of an aldehyde alkenyl chloride compound; and 2) adjusting the pH value of the aldehyde alkenyl chloride compound prepared in the step 1) and hydrazine hydrate or hydrazine salt to 2-10, reacting at 10-60 DEG C, adding an alkaline substance to adjust the pH valueto 6-11 after the reaction is completed, and carrying out post-treatment to obtain the 3, 4-dimethylpyrazole. According to the preparation method, by reacting the 2-butanone, phosphorus oxychloride and N, N-dimethylformamide to obtain the alkenyl chloride compound, reacting the alkenyl chloride compound with the hydrazine hydrate or hydrazine salt, carrying out post-treatment to obtain the 3, 4-dimethylpyrazole, and salifying the 3, 4-dimethylpyrazole and phosphoric acid, the 3, 4-dimethylpyrazole phosphate is obtained. The method is cheap and easily available in raw material, short in step, simple and convenient to operate, high in yield, high in product quality and suitable for industrial production, and the solvent can be recycled.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a preparation method of 3,4-dimethylpyrazole and its phosphate. Background technique [0002] 3,4-Dimethylpyrazole phosphate (DMPP) is a nitrogen fertilizer nitrase inhibitor developed by BASF in Germany. It has the characteristics of high efficiency, non-toxicity, stability and specificity. DMPP can significantly inhibit soil NH 4+ -N to NO 3- -N conversion, showing significant nitrification inhibition effect, and far superior to similar products (Journal of Plant Nutrition and Fertilizer, 2017, 23, 54). Since the field application test in Germany and Europe in 1999, it has been successfully commercialized and applied to agricultural production on a large scale. Therefore, it is also known as the most promising new generation of slow-release fertilizer in the 21st century. Broad application prospects. [0003] 3,4-dimethylpyrazole is an important intermediate in the synthes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D231/12
CPCC07D231/12
Inventor 于亦忠高于王志浩国洪雷施裕华
Owner 武威金仓生物科技有限公司
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