The invention discloses a preparation method of 3-chloro-5, 5-dimethyl-4, 5-dihydroisoxazole, which comprises the following steps: taking a
hydroxylamine oxygen sulfonic acid aqueous solution and isopentenal as raw materials, carrying out oximation reaction in an
organic solvent under an alkaline condition, then directly adding an acid or an
organic base catalyst into the
reaction system, and reacting for 2-4 hours to obtain 3-chloro-5, 5-dimethyl-4, 5-dihydroisoxazole, thereby obtaining the 3-chloro-5, 5-dimethyl-4, 5-dihydroisoxazole. Under the catalytic action of the catalyst, a cyclization reaction is carried out, after the reaction is finished, an intermediate solution containing 5, 5-dimethyl-4, 5-dihydroisoxazole is obtained, and the next step is directly carried out; and carrying out a chlorination reaction by taking the intermediate solution as a
raw material and
sodium hypochloride or
chlorine as a chlorination
reagent, and after the reaction is finished, carrying out post-treatment to obtain the 3-chloro-5, 5-dimethyl-4, 5-dihydroisoxazole. The
hydroxylamine oxygen sulfonic acid is used for enabling the isopentenal to be subjected to oximation reaction under the alkaline condition, then cyclization is carried out under the catalytic action of acid or alkali, the 5, 5-dimethyl-4, 5-dihydroisoxazole is generated, and the process has the advantages that the yield is high, the production steps are simplified, and the production cost is reduced.