Study on the Synthesis of 4,4-dimethylisoxazole-3-one
In order to increase the yield of 4,4-dimethyl isoxazoL-3-one and save the experimental cost,a better experimental synthesis method was discussed on the basis of previous studies.In this paper,4,4-dimethylisoxazole-3-ketone was produced by oxime and cyclization reaction u-sing tervaloyl chloride and hydroxylamine hydrochloride as starting materials,water as solvent and NaOH as acid binding agent.Orthogonal ex-periment was used to optimize the synthesis conditions of reactant feeding ratio,reaction time,acid binding concentration and reaction tempera-ture.The results showed that the oximation reaction at 0-15 ℃ could inhibit the decomposition of hydroxylamine hydrochloride and tervaloyl chloride.The reaction ratio was 1∶1.3,the concentration of sodium hydroxide was 30％,the reaction time was 3 h,the ring formation reaction lasted for 18-20 h,and the yield was 64.84％.
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