4,4-二甲基异噁唑-3-酮的合成研究  

Study on the Synthesis of 4,4-dimethylisoxazole-3-one

作　　者：谢耀濂 唐依萍 刘英 李致宝 郭洋洋[1] Xie Yaolian;Tang Yiping;Liu Ying;Li Zhibao;Guo Yangyang(Guangxi Normal University for Nationalities,Chongzuo 532200,China)

机构地区：[1]广西民族师范学院,广西崇左532200

出　　处：《云南化工》2024年第11期42-45,共4页Yunnan Chemical Technology

基　　金：广西民族师范学院2024年特色本科高校建设项目—制药工程(项目编号:395003010109);广西壮族自治区级大学生创新创业训练计划项目(项目编号:S202410604109)。

摘　　要：为了提高4,4-二甲基异噁唑-3-酮的产率,节约实验成本,在前人所研究的基础上,探讨其更为优质的实验合成方法。以氯代特戊酰氯和盐酸羟胺为起始原料,水为溶剂,NaOH为缚酸剂,经过肟化、环合反应生成4,4-二甲基异噁唑-3-酮,采用正交实验法对反应物投料比、反应时间、缚酸剂浓度、反应温度等各方面合成条件进行优化。结果表明,肟化反应在0~15℃的温度下进行,可抑制盐酸羟胺与氯代特戊酰氯的分解,反应投料比为1∶1.3,氢氧化钠质量分数为30%,反应时间为3 h,成环反应进行18~20 h,收率为64.84%。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 using tervaloyl chloride and hydroxylamine hydrochloride as starting materials,water as solvent and NaOH as acid binding agent.Orthogonal experiment was used to optimize the synthesis conditions of reactant feeding ratio,reaction time,acid binding concentration and reaction temperature.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%.

关 键 词：4 4-二甲基异噁唑-3-酮 氯代特戊酰氯 盐酸羟胺 肟化反应 环合反应 

分 类 号：TQ452.2[化学工程—农药化工]