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A kind of preparation method of paclobutrazol

A technology of paclobutrazol and compounds, applied in the field of preparation of paclobutrazol, can solve the problems of low yield, large amount of three wastes, expensive reagents, etc., and achieve the effects of high content and yield, simple operation, and low cost

Active Publication Date: 2021-12-28
JIANGSU SEVENCONTINENT GREEN CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above-mentioned reduction system is either expensive in reagent price, high in cost, low in yield, high in the ratio of isomers, and there are also unfavorable factors such as a large amount of three wastes.
Invention CN103664809B discloses a method for preparing paclobutrazol by formula (I) under the hydrogen / palladium-carbon reduction system, and the yield is ideal, but the cost of palladium-carbon is expensive, and there are serious potential safety hazards when it is applied on a large scale in industrialization

Method used

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  • A kind of preparation method of paclobutrazol
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  • A kind of preparation method of paclobutrazol

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Add 150g methanol, 50g formula (I) represented compound, 5g Raney nickel in the hydrogenation reactor. First replace with nitrogen three times, then replace with hydrogen three times, keep the hydrogen pressure at 2.0 MPa, then start stirring, and heat the reaction system to 50°C for 3 hours. Sampling HPLC analysis formula (I) after the content of the compound represented by the formula (I) is less than 1%, stop the reaction, filter the material to remove solid insolubles, after the filtrate reclaims most of the methanol, cool and crystallize, filter and dry to obtain 49.72g light yellow solid, which is Paclobutrazol, content 96.2%, yield 95.0%.

Embodiment 2

[0024] In the hydrogenation reactor, add 160g ethanol, the compound represented by 50g formula (I), 0.5g Raney nickel. First replace with nitrogen three times, then replace with hydrogen three times, keep the hydrogen pressure at 4.0MPa, then start stirring, and heat the reaction system to 60°C for 5 hours. After the compound represented by HPLC analysis formula (I) is less than content 1%, stop the reaction, filter the material to remove solid insolubles, after the filtrate reclaims most of the ethanol, cool and crystallize, filter and dry to obtain 50.12g light yellow solid, which is Paclobutrazol, content 95.7%, yield 95.3%.

Embodiment 3

[0026] Add 180g isopropanol, the compound represented by 50g formula (I) and 2.0g Raney nickel in the hydrogenation reactor. First replace with nitrogen three times, then replace with hydrogen three times, keep the hydrogen pressure at 4.0MPa, then start stirring, and heat the reaction system to 50°C for 4.5 hours. Sampling HPLC analysis formula (I) after the compound content represented by formula (I) is less than 1%, stop reaction, material is filtered and removed solid insoluble matter, after filtrate reclaims most of isopropanol, crystallization by cooling, drying by filtration, obtains 50.01g pale yellow solid, That is paclobutrazol with a content of 96.5% and a yield of 95.8%.

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Abstract

The invention relates to a preparation method of paclobutrazol. The preparation method uses a compound represented by formula (I) as a raw material to carry out catalytic hydrogenation reaction in the presence of hydrogen and a catalyst, thereby preparing paclobutrazol. Wherein, the chemical name of the compound represented by formula (I) is 1-(4-chlorophenyl)-4,4-dimethyl-2-[1,2,4-triazolyl]-1-pentene- 3-ketone. The process of the invention is relatively safe, simple in operation, low in cost, less in three wastes, higher in paclobutrazol content and yield, and suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of paclobutrazol. Background technique [0002] Paclobutrazol, the chemical name is (2RS, 3RS)-1-(4-chlorophenyl)-4,4-dimethyl-4-(1H-1,2,4-triazol-1-yl) Pent-3-ol is a widely used plant growth regulator and has fungicidal activity. It was first developed and promoted by the British Imperial Chemical Industries Group. The agricultural application value of paclobutrazol lies in its control effect on crop growth, which has the effects of delaying plant growth, inhibiting stem elongation, shortening internodes, promoting plant tillering, promoting flower bud differentiation, increasing plant stress resistance, and increasing yield. It is suitable for rice, wheat, peanuts, fruit trees, tobacco, rape, soybeans, flowers, lawns and other crops (plants), and the effect is remarkable. [0003] Since paclobutrazol plays an important role in agricultural production, its preparation method is very important. Most of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D249/08
CPCC07D249/08
Inventor 张虎吕国雨周志豪徐秋龙盛莹盈
Owner JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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