Method for synthesizing pyraclostrobin intermediate
2016
The invention discloses a method for synthesizing a pyraclostrobin intermediate. The synthetic method comprises the following steps: preparing an intermediate 1-(4-chlorophenyl)-3-hydroxy-1-h-pyrazole from 4-chlorophenylhydrazine hydrochloride prepared with p-bromochlorobenzene and hydrazine hydrate as reaction raw materials; reacting o-nitrotoluene with chlorine in the presence of a catalyst so as to prepare o-nitrobenzyl chloride; and subjecting 1-(4-chlorophenyl)-3-hydroxy-1-h-pyrazole and o-nitrobenzyl chloride to an etherification reaction so as to obtain the pyraclostrobin intermediate, i.e., an etherification product 2[(N-4-chlorophenyl)-3-pyrazolyl-oxymethyl]nitrobenzene. The synthetic method provided by the invention can greatly reduce the amount of waste water produced in the synthesis process of 4-chlorophenylhydrazine hydrochloride; with 4-chlorophenylhydrazine hydrochloride as a raw material, the produced intermediate 1-(4-chlorophenyl)-3-hydroxy-1-h-pyrazole has HPLC content of no less than 98% and yield of no less than 90%; since chlorine is used for replacing bromine or hydrobromic acid to prepare o-nitrobenzyl bromide, production cost and environmental protection burden are controlled; and the etherification product with a content of no less than 98% and yield of no less than 90% is obtained.
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