The invention discloses a synthesis method of
diisopropyl azodicarboxylate. The synthesis method comprises the following steps: (1) adding alkali and a
solvent under protection of
inert gases, sequentially adding carbazic acid
isopropyl ester and
diethyl carbonate, carrying out heating reaction at 100-180 DEGC for 2-6 hours, adjusting the pH value of a solution to 4.5-7.5 with acid, and carrying out suction
filtration, so as to obtain hydrogenated diisopropyl azodiformate; and (2) adding 40%-50% of
sulfuric acid solution to the hydrogenated diisopropyl azodiformate at -20 DEG C to 25 DEG C, dissolving, adding a catalyst, controlling the
reaction temperature to -15 DEG C to -5 DEG C, dropwise adding 10%-15% of
hydrogen peroxide until no heat is emitted, further reacting for 5-10 hours after dropwise adding is ended,
quenching, extracting, washing to be neutral,
drying, filtering, and concentrating to obtain the diisopropyl azodiformate. The synthesis method disclosed by the invention is clean and environmental friendly in
raw material, mild in reaction condition, and few in byproducts; and the product is high in yield and beneficial to industrialized production.