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Method for synthesizing azaconazole through 4-amino-4H-1,2,4-triazole alkylation

A technology of -4H-1 and triazolidine, which is applied in the preparation of carbon-based compounds, chemical instruments and methods, and the preparation of organic compounds, can solve problems such as difficult operation and high price

Inactive Publication Date: 2018-10-19
QILU NORMAL UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

But these methods are either difficult to operate or expensive

Method used

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  • Method for synthesizing azaconazole through 4-amino-4H-1,2,4-triazole alkylation
  • Method for synthesizing azaconazole through 4-amino-4H-1,2,4-triazole alkylation
  • Method for synthesizing azaconazole through 4-amino-4H-1,2,4-triazole alkylation

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Embodiment Construction

[0102] The present invention is carried out like this, a kind of synthetic method of penconazole intermediate, mainly is the synthetic method of 2,4-dichloroacetophenone, 2-bromo-1-(2,4-dichlorophenyl) Synthetic method of ethyl ketone and synthetic method of ketal.

[0103] 2, the synthetic method of 4-dichloroacetophenone, concrete steps are:

[0104] (1) In a 250ml three-necked bottle, install a stirrer at the middle port, install a dropping funnel and a condenser tube at the two ports, install a calcium chloride drying tube at the upper end of the condenser tube, and connect a hydrogen chloride gas absorption device;

[0105] (2) Quickly weigh 20g (0.15 mol) of anhydrous aluminum trichloride powder, put it into a three-necked bottle, then add 30 ml m-dichlorobenzene, add 6 ml (0.06 mol) acetic anhydride dropwise under stirring, about 20 minutes to finish dripping;

[0106] (3) Then keep boiling slightly on the heating mantle for half an hour until no hydrogen chloride gas...

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Abstract

The invention discloses a method for synthesizing azaconazole through 4-amino-4H-1,2,4-triazole alkylation. The method comprises step 1, preparing a raw material which is shown in a following image; step 2, synthesizing 1-(2,4-dichlorophenyl)-2-(1H-1,2,4-triazole-1-yl) ethanone; step 3, synthesizing azaconazole. The method disclosed by the invention has the advantages that development of a novel azaconazole bactericide successfully fills the blank in China, synthesis researches of similar derivatives based on the azaconazole bactericide will be in the ascendant, and successful development andindustrial implementation of varieties of novel bactericides have a far-reaching influence on national economy development. The method disclosed by the invention is an azaconazole synthesizing method.

Description

technical field [0001] The invention relates to the field of penconazole, in particular to a method for synthesizing penconazole by alkylation of 4-amino-4H-1,2,4-triazole. Background technique [0002] Azaconazole (azaconazole), its structural formula is , is a new type of fungicide. The present invention uses various methods to explore and study the synthesis of penconazole. At the same time, due to the unique structure and excellent performance of the zeolite catalyst, it is also used in the synthesis of its intermediate brominated ketal. [0003] First, we use p-toluenesulfonic acid as a catalyst to prepare the intermediate bromoketal and chlorinated ketal of penconazole in benzene, benzene+butanol, toluene, and xylene respectively. We found that the yield of brominated ketals was always greater than that of chloroketals in any solvent. Among various solvents, the reaction yield in benzene+butanol is the highest whether it is brominated ketal or chlorinated ketal. ...

Claims

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Application Information

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IPC IPC(8): C07D405/06C07C45/00C07C49/807C07C45/63C07C49/80C07D317/16B01J29/08B01J37/30B01J37/08B01J37/10
CPCB01J29/084B01J37/08B01J37/10B01J37/30B01J2229/16C07C45/00C07C45/63C07C49/80C07C49/807C07D317/16C07D405/06
Inventor 刘忠强
Owner QILU NORMAL UNIV
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