Analysis of by-products formation in the synthetic processes of prothioconazole
Some side reactions in the synthetic processes of prothioconazole led to by-products.They negatively affect the yield and quality of prothioconazole.Three different synthetic processes were investigated.Four by-products,including 2-(1-chlorocyclopropyl)-1-(2-chlorophenyl)-3-(4H-1,2,4-triazol-4-yl)propan-2-ol(7),6-(2-chlorobenzyl)-6-(1-chlorocyclopropyl)-5,6-dihydro-4H-1,3,4-oxadiazine-4-carbothioamide(8),dimer-prothioconazole(9)and 2-(2-chlorobenzyl)-2-((5-thioxo-4,5-dihydro-1,2,4-triazol-1-yl)methyl)cyclobutanone(10),were synthesized and characterized by 1H NMR,13C NMR,ESI-MS or X-Ray diffraction.Among them,the by-product 8 was first discovered during the synthesis of prothioconazole by substituting hydrazine-acetone.The study revealed the mechanism of generation of the four by-products in different processes.The results provided an important guide for the selection and control of the synthetic process of prothioconazole and product quality improvement.
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