Study On The Synthesis Of Flusilazole

Flusilazole belongs to Triazole fungicides.It is inhibitor of sterol demethylation.Itprovides excellent control of a broad spectrum of diseases on a wide rang of economicallyimportant crops.The fungicide has a high bactericidal activity,fast bactericidal，smalldosage,low toxicity to animals,at the same time,it has good selectivity for beneficial insects.This paper reviews the preparation of flusilazole and its importantintermediate.Analyze the correlated literature and design the route of flusilazole.FirstGrignard reagent was prepared from1-bromo-4-fluorobenzene and magnesium in tolueneand THF.Second the(Chloromethyl)bis4-fluorophenylmethylsilane was synthesized byGrignard reagent and dichlorochloromethylmethylsilane.Finally the title compoundflusilazole was synthesized from (Chloromethyl)bis4-fluorophenylmethylsilane with1,2,4-triazole sodium salt.In the process of preparing of(Chloromethyl)-bis4-fluorophenylmethylsilane,we analysised the main impurities in thereaction,and combined experimental result confirmed the structure of the impurity.The results show that the purity of the Grignard reagent was95.6%when the reactionsolvent was toluene and tetrahydrofuran,the volume ratio of1-bromo-4-fluorobenzene andthe solvent was1:5,the material ratio was1:1.3and reaction temperature was35℃in thesynthesis of Grignard reagent.the yield was88.7%when the material ratio was1:1.05,reaction temperature was25℃and the concentration of hydrochloric acid was5%in the synthesis of (Chloromethyl)bis4-fluorophenylmethylsilane.the yield was98.8%andthe purity was more than90%in the synthesis of1,2,4-triazole sodium salt, the yield was72.8%and the purity was more than95.8%when the material ratio was1:1.1,reactiontemperature was85℃and reaction time was5h in the synthesis of flusilazole.