PEG400-PdCl_2催化合成频那酮  

Catalytic Synthesis of Pinacolone with PEG400-PdCl_2

作　　者：胡佳佳[1] 倪雷清 陆国太 万家文 林陵[1] 曾崇余[1] 

机构地区：[1]南京工业大学化工学院,南京210009

出　　处：《农药》2016年第6期396-399,共4页Agrochemicals

基　　金：江苏高校品牌专业建设工程资助项目(PPZY2015A044)

摘　　要：[目的]提高频那酮收率,减少废酸生成。[方法]以PEG400-Pd Cl_2为催化剂,用三聚甲醛(1,3,5-三氧杂环己烷)替代甲醛溶液与2-氯-2-甲基丁烷在盐酸中合成频那酮(3,3-二甲基-2-丁酮)。较优条件:n(Pd Cl_2)∶n(2-氯-2-甲基丁烷)为3∶100,n(PEG400)∶n(Pd Cl_2)为1∶1,盐酸质量分数为26%,n(三聚甲醛)∶n(2-氯-2-甲基丁烷)为0.45∶1,反应时间为8 h,反应温度为85℃。[结果]频那酮收率达到76.8%。[结论]三聚甲醛替代甲醛溶液减少了反应中废酸的生成,反应中使用PEG400-Pd Cl_2催化剂使得频那酮收率得到提高。[Aims] This paper aims to enhance the yield of pinacolone and reduce the production of waste acid.[Methods] Using PEG400-PdCl_2 as catalyst, trioxymethylene instead of formaldehyde was reacted with2-chloro-2-methylbutane to produce pinacolone in the presence of hydrochloric acid solution. The optimized conditions were as follows： the molar ratio of PdCl_2 and 2-chloro-2-methylbutane was 3∶100, the molar ratio of PEG400 and PdCl_2 was 1 ∶1, the mass fraction of hydrochloric acid solution was 26%, the molar ratio of trioxymethylene and 2-chloro-2-methylbutane was 0.45 ∶1, the reaction time was 8 h, the reaction temperature was 85 ℃. [Results] The yield of pinacolone was 76.8% under optimized conditions. [Conclusions] The method using trioxymethylene to replace formaldehyde solution to produce pinacolone can reduce the production of waste acid greatly. The yield of pinacolone was improved by using PEG400-PdCl_2 catalyst.

关 键 词：频那酮 三聚甲醛 2-氯-2-甲基丁烷 PEG400-Pd CL2 

分 类 号：O623.52[理学—有机化学] TQ450.4[理学—化学]