The invention discloses a preparation method of 3, 4, 5, 6-tetrafluorophthalonitrile, and belongs to the technical field of organic intermediates. The preparation method comprises the following steps: reacting 3, 4, 5, 6-tetrafluorophthalic dicarboxaldehyde serving as a
raw material with
hydroxylamine hydrochloride to generate a dioxime intermediate; the preparation method comprises the following steps: reacting 2, 4, 5, 6-tetrafluorophthalonitrile with 1, 3-
benzene disulfonyl
chloride to generate a cyclized intermediate, and finally removing 1, 3-
benzene disulfonic acid to generate 3, 4, 5, 6-tetrafluorophthalonitrile. According to the method, the design is reasonable, the yield is high, the cyclization intermediate does not need to be purified, the dinitrile product can be obtained through
catalysis of a small amount of acid, and a convenient
route is provided for high-yield obtaining of high-quality 3, 4, 5, 6-tetrafluorophthalonitrile.