The invention discloses a preparation method of pyridinetriazolone, and belongs to the technical field of
organic synthesis, and the preparation method comprises the following steps: taking hydrazine
hydrate as a starting
raw material, adding
urea in batches at the temperature of 80-85 DEG C, carrying out heat preservation reaction to obtain
semicarbazide, dropwise adding
hydrochloric acid to form salt, and
drying under reduced pressure to obtain
semicarbazide hydrochloride; adding the
semicarbazide hydrochloride obtained in the previous step and 2-chloropyridine into an
ethylene glycol
monomethyl ether system, heating to 130-135 DEG C, refluxing, adding a catalytic amount of concentrated
sulfuric acid, and carrying out heat preservation reaction to obtain
pyridine triazolone; and
drying the post-treated
mother liquor under reduced pressure, weighing, adding quantitative
urea, heating to 130-135 DEG C, and reacting to obtain the
pyridinium triazolone. The initial raw materials are hydrazine
hydrate and
urea, are common industrial raw materials, are easy to obtain and low in price, and are beneficial to industrial production; the by-product 2-hydrazinopyridine is recovered and reacts with urea to prepare the pyridintriazolone, so that the
raw material utilization rate and the product yield are greatly improved, the total yield reaches more than 80%, and the purity of the pyridintriazolone is more than or equal to 99.0%.