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Preparation method for paclobutrazol

A technology of paclobutrazol and reaction, which is applied in the direction of organic chemistry, can solve the problems of large environmental pollution, etc., and achieve the effect of no environmental pollution and simple reaction process

Active Publication Date: 2014-03-26
JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] This report adopts sodium hydroxide aqueous solution as acid-binding agent when synthesizing the compound represented by formula (III), and the synthesis process produces a large amount of sodium chloride alkaline waste water, which causes great environmental pollution.

Method used

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  • Preparation method for paclobutrazol
  • Preparation method for paclobutrazol
  • Preparation method for paclobutrazol

Examples

Experimental program
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Embodiment 1

[0026] This embodiment provides a preparation method of a compound represented by formula (I), the specific implementation is as follows:

[0027] Add 7.99g (0.11mol) of 1,2,4-triazole, 8.45g (0.06mol) of potassium carbonate and 45g of ethanol to the reaction flask, heat to 60°C, then add 14.15g (0.1mol) dropwise over 1 hour ) α-chloropinacolone into the reaction bottle, after the dropwise addition, react at 60°C for 3 hours, and then take a sample for GC analysis. When the α-chloropinacolone is less than 1%, the reaction is terminated. The reaction liquid is cooled and filtered to recover potassium carbonate, after the filtrate recovers ethanol under normal pressure, the residue 18g is the compound represented by formula (II), then add 60g toluene, 13.7g (0.095mol) p-chlorobenzaldehyde, 1g trichlorobenzaldehyde to the filtrate Ethylamine, heated to 120°C, dehydrated with toluene reflux for 4 hours, sampled for GC analysis, when the p-chlorobenzaldehyde was less than 1%, the r...

Embodiment 2

[0029] The present embodiment provides a kind of preparation method of paclobutrazol, concrete implementation is as follows:

[0030] Add 90g of methanol, 30g (0.094mol) of the compound represented by formula (I) and 16.21g (0.3mol) of ammonium chloride to the reaction flask, stir and heat to 40°C, add 3.64g (0.15mol) in batches within half an hour ) magnesium powder, then react at 50°C for 1 hour, and absorb the ammonia gas released during the reaction with water. Sampling GC analysis formula (I) after the compound is less than 1%, the material is filtered to remove magnesium chloride, after the filtrate reclaims part of methanol, cooling and crystallization, filtration and drying, to obtain 26.2g off-white solid, which is paclobutrazol, content 96.2%. The rate is 91.4%.

Embodiment 3

[0032] The present embodiment provides a kind of preparation method of paclobutrazol, concrete implementation is as follows:

[0033] Add 120g of ethanol, 30g (0.094mol) of the compound represented by formula (I) and 21.61g (0.4mol) of ammonium chloride to the reaction flask, stir and heat to 50°C, add 4.85g (0.2mol) in batches within half an hour ) magnesium powder, then react at 60°C for 2 hours, and absorb the ammonia gas released during the reaction with water. Sampling GC analysis formula (I) after the compound is less than 1%, the material is filtered to remove magnesium chloride, after the filtrate reclaims part of the ethanol, cooling and crystallization, filtering and drying, obtain 26.4g off-white solid, which is paclobutrazol, content 96.1%. The rate is 91.9%.

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Abstract

The invention relates to a preparation method for paclobutrazol. The preparation method comprises a step of subjecting a compound represented by a formula (I) to a reduction reaction under the action of a reducing agent so as to produce paclobutrazol; in the reduction reaction, the two function groups consisting of a double bond and a carbonyl group on the chain of the compound represented by the formula (I) are reduced into a single bond and a hydroxyl group, and paclobutrazol is obtained in one step; the chemical name of the compound represented by the formula (I) is 1-(4-chlorophenyl)-4,4-dimethyl-2-[1,2,4-triazolyl]-1-pentene-3-one. The preparation method provided by the invention has the advantages of simple process, convenient operation, high reaction yield, low production cost and no generation of waste water.

Description

technical field [0001] The invention relates to a preparation method of paclobutrazol. Background technique [0002] The chemical name of paclobutrazol is (2RS,3RS)-1-(4-chlorophenyl)-4,4-dimethyl-2-(1H-1,2,4-triazol-1-yl)pentan-3 -Alcohol, the original drug is a white solid. Paclobutrazol (Propiconazole) is a triazole plant growth regulator and an inhibitor of endogenous gibberellin synthesis. It has the functions of delaying plant growth, inhibiting stem elongation, shortening internodes, promoting plant tillering, promoting flower bud differentiation, and increasing plant growth. Anti-stress performance, increase production and other effects. This product is suitable for rice, wheat, peanuts, fruit trees, tobacco, rapeseed, soybeans, flowers, lawns and other crops (plants), and the use effect is remarkable. [0003] "Jiangsu Agricultural Science" reported the preparation method of paclobutrazol in the S1 phase of 1987. The method uses α-chloropinacolone as a starting m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D249/08
CPCC07D249/08
Inventor 陶伟韩士芳吕宜飞龚建华苏镜
Owner JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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