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Preparation method of 3,4-dimethylpyrazole and preparation method of 3,4-dimethylpyrazole phosphate

A technology of dimethylpyrazole phosphate and dimethylpyrazole, which is applied in the chemical field, can solve the problems of limited promotion, high cost of raw materials, harsh reaction conditions, etc., and achieve cheap and easy-to-obtain raw materials, high-quality products, and easy operation Effect

Pending Publication Date: 2019-09-10
武威金仓生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it needs to use extremely flammable alkali metal sodium, which is extremely dangerous and not suitable for large-scale amplification
Simultaneously the use of ether has also limited the popularization of this method
[0010] There are many synthetic routes in the above-mentioned public reports, but there are many shortcomings, such as high cost of raw materials, harsh reaction conditions, extremely flammable dangerous reagents involved, serious environmental pollution and other problems, which are not conducive to large-scale industrial production

Method used

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  • Preparation method of 3,4-dimethylpyrazole and preparation method of 3,4-dimethylpyrazole phosphate
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Examples

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Effect test

Embodiment 1

[0048] Example 1 Preparation of 1-dimethylamino-2-methyl-1-buten-3-one

[0049] Add 60g of 2-butanone, 100g of methyl formate and 400g of toluene into the reaction flask, add 81g of sodium methoxide solid in batches under control of the internal temperature at 0-15°C, and then react at 10-35°C for 4 hours. Add 30% aqueous solution of dimethylamine hydrochloride (88g of dimethylamine hydrochloride dissolved in 205g of water) to the reaction solution at 15-35°C, react at 10-35°C for 3 hours after the dropwise addition is completed, and then separate the layers. The aqueous phase was extracted once with toluene, and the organic layers were combined and concentrated to obtain an oil.

Embodiment 2

[0050] Example 2 Preparation of 3,4-dimethylpyrazole

[0051] Add the 1-dimethylamino-2-methyl-1-buten-3-one prepared in Example 1 into a three-necked flask, slowly add 52 g of 80% hydrazine hydrate solution dropwise, and then control the temperature at 15-35°C Slowly add hydrochloric acid dropwise to adjust the pH value to 7-9, keep the reaction at 15-45°C for 2 hours, slowly add 20% NaOH aqueous solution dropwise to adjust the pH value to 7-10, add 140g toluene, and statically separate to obtain an organic layer , the solvent was distilled off under reduced pressure to obtain the crude product 3,4-dimethylpyrazole with a yield of 79%, which could be directly used in the next step of salt formation.

Embodiment 3

[0052] Example 3 Preparation of 3,4-dimethylpyrazole phosphate

[0053] Dissolve the 3,4-dimethylpyrazole obtained in Example 2 in 144g of methanol, add 96g of 85% phosphoric acid at room temperature to adjust the pH value to 3-7, continue to stir and react at 15-25°C for 2 hours, filter, and dry. 110 g of 3,4-dimethylpyrazole phosphate white solid was obtained, with a total yield of 68%. 1H NMR (400MHz, DMSO-d6) δ=11.03(brs,4H),7.26(s,1H),2.10(s,3H),1.91(s,3H).

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Abstract

The invention discloses a preparation method of 3,4-dimethylpyrazole and a preparation method of 3,4-dimethylpyrazole phosphate. The methods comprise the following steps: performing condensation by using 2-butanone and formate as raw materials, performing aminolysis, performing cyclization to prepare the 3,4-dimethylpyrazole; and performing a salt forming reaction on the 3,4-dimethylpyrazole and phosphoric acid to obtain the 3,4-dimethylpyrazole phosphate. The preparation method of the 3,4-dimethylpyrazole and the preparation method of the 3,4-dimethylpyrazole phosphate provided by the invention have the significant advantages that the raw materials are cheap and easy to obtain, the operation is simple and convenient, the yield is high, the product quality is high, the solvent can be recovered and reused, and the methods are suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemistry and relates to a preparation method of 3,4-dimethylpyrazole and 3,4-dimethylpyrazole 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. Studies have shown that 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 a...

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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