85491-26-5Relevant articles and documents
Flusilazole and synthesis method thereof
-
Paragraph 0033-0038; 0043-0044; 0048-0049; 0053-0054, (2018/12/14)
The invention discloses flusilazole and a synthesis method thereof. The synthesis method comprises the following steps: putting magnesium powder into a Grignard reaction kettle; adding an organic solvent and uniformly stirring; cooling and adding p-fluorobromobenzene in one step; mixing and stirring; dropwise adding the p-fluorobromobenzene, and keeping heat and reacting; cooling and storing to obtain a p-fluorobromobenzene Grignard reagent; raising the temperature of the p-fluorobromobenzene Grignard reagent; dropwise adding methyl chloromethyl dichlorosilane and carrying out heat insulation;recycling an organic solvent under negative pressure to obtain a flusilazole intermediate, magnesium bromide and magnesium chloride; adding DMF (Dimethyl Formamide), stirring, cooling and centrifuging; removing the magnesium bromide and the magnesium chloride to obtain a DMF mother solution; dissolving triazole sodium salt into formamide; adding the DMF mother solution and reacting; recycling theDMF under negative pressure and distilling in vacuum; cooling to obtain the flusilazole. The content of the flusilazole is greater than or equal to 95.0 percent and the yield is 80 to 90 percent; thesynthesis method has the advantages of moderate reaction conditions, safety in operation, low equipment requirements, low cost, no wastewater and easiness for operation and implementation, and is suitable for large-scale production of enterprises.