Method for synthesizing azaconazole bactericide through reaction between bromo ketal and 1H-1,2,3-triazole

A technology of penticonazole and fungicide, which is applied in the field of synthesizing penticonazole fungicide by reacting bromo ketal and 1H-1,2,4-triazole, and can solve the problems of difficult operation and high price.

Inactive Publication Date: 2018-10-19
QILU NORMAL UNIV
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  • Method for synthesizing azaconazole bactericide through reaction between bromo ketal and 1H-1,2,3-triazole
  • Method for synthesizing azaconazole bactericide through reaction between bromo ketal and 1H-1,2,3-triazole
  • Method for synthesizing azaconazole bactericide through reaction between bromo ketal and 1H-1,2,3-triazole

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[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 bactericide through reaction between bromo ketal and 1H-1,2,3-triazole. The method comprises partial steps: putting 1.15g of sodium (0.05mol) into a 250 ml three-neck flask containing 60 ml of methyl alcohol, adding 3.45g (0.05 mol) of 1H-1,2,4-triazole after reaction is completed, stirring for 30 minutes under the room temperature, adding 75 ml of N,N-dimethyl formamide and evaporating to remove the methyl alcohol under the normal pressure until a temperature in the flask reaches 130 DEG C. The method disclosed by the invention has the advantages that azaconazole novel bactericide development successfully fills a gap in China, synthesis researches of similar derivatives based on the azaconazole bactericide will be in the ascendant, and successful development and industrial implementation of varieties of novel bactericides have a far-reaching influence on national economy development. The method disclosed by the invention is a novel azaconazole synthesizing method.

Description

technical field [0001] The invention relates to the field of penconazole, in particular to a method for synthesizing a penconazole fungicide by reacting a brominated ketal with 1H-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 ...

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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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