Improvement On Synthesis Process Of Chlorantraniliprole And Fluconazole’s Intermediates

Pesticides generally refer to chemicals and biopharmaceuticals which used to control harmful organisms and to regulate plant growth.Since ancient times,in order to meet the needs of people’s agricultural production,pesticide products have been undergoing renewal and optimization,and there are more and more pesticide varieties.However,the use of a large number of pesticides has seriously affected the human natural environment.Old,high-toxic and high-residue pesticides have been phased out.The development of green,low-toxic,and environmentally friendly new pesticides has gradually become the focus of research.Fluconazole and chlorantraniliprole have good market prospects,but the problems of low yield and high pollution have been limiting their industrialization process.In view of the problems in the synthesis process,the synthesis process and process of key intermediates of chlorantraniliprole and fluconazole are studied in this paper.In the research on the synthesis process of chlorantraniliprole intermediates,this a rticle established high-performance liquid analysis methods for the 3-bromo-1-(3-chloro-2-pyridyl)-1H-pyrazole-5-carboxylic acid and chlorantraniliprole compounds.Make 2,3-dichloropyridine as the raw material in the experiment,after reaction with hydrazine h ydrate to get 3-chloro-2-hydrazinopyridine,after cyclization reaction with diethyl maleat e to get 2-(3-chloro-2-pyridyl)-5-pyrazolidinone-3-carboxylic acid ethyl ester,after bro mination reaction to get 3-bromo-1-(3-chloropyridin-2-pyridyl)-4,5-Dihydro-1H-pyrazole-5-carboxylic acid ethyl ester,and then through oxidation reaction to get 3-bromo-1-(3-chloro-2-pyridyl)-1H-pyrazole-5-carboxylic acid Ethyl ester,and finally through hydroly zed to get 3-bromo-1-(3-chloro-2-pyridyl)-1H-pyrazole-5-carboxylic acid.In this chapter,the influencing factors such as reaction time,reaction temperature,reactant ratio,cata lyst and solvent were tested and discussed one by one.Finally,the best synthesis pro cess was determined.In the research on the synthesis process of fluconazole intermediates,this article established high-performance liquid analysis methods for the p-chloro-3-(2-chlorophenyl)-2-(4-fluorophenyl)-2-propanol,Z-1-chloro-3-(2-chlorophenyl)-2-(4-fluorophenyl)-2-propen e and E-1-chloro-3-(2-chlorophenyl)-2-(4-fluorophenyl)-2-propene.And through the two methods of alcohol dehydration and cis-reversion to improve the yield of Z-isomer.U nder the optimal conditions,the solid superacid catalyzed the dehydration of alcohol t o obtain the Z-isomer with a yield of 69.6%.Under the optimal conditions,the cataly st catalyzed the conversion of Z/E to obtain the Z-isomer with a yield of 69.4%.By the difference in the melting points of the Z and E isomers in the solvent at low te mperatures,more Z isomers can be obtained in the Z/E mixture.