2-烯丙基-1,3-二苯基-1,3-丙二酮的制备工艺条件的优化

摘要

以聚乙二醇-600为相转移催化剂,通过正交实验研究了3-溴丙烯和1,3-二苯基-1,3-丙二酮(DPP)物质的量之比(B/D)、聚乙二醇-600和DPP物质的量之比(P/D)、反应时间(t)、反应温度(T)等因素对2-烯丙基-1,3-二苯基-1,3-丙二酮(ADPP)产率的影响,得出制备ADPP的最佳工艺条件为:B/D=1.1,P/D=0.10%,t=6 h,T=50 ℃;在此条件下,所得产物经IR,1H NMR,MS 和元素分析确认为ADPP的结构,且ADPP产率达86.3%.%The effects of mole ratio of 3-bromo-1-propene and 1,3-diphenyl-1,3-propanedione(DPP)(B/D),mole ratio of PEG-600 and DPP(P/D),reaction time(t)and temperature(T)on the yield of 2-allyl-1,3-diphenyl-1,3-propanedione (ADPP)with PEG-600 as the phase transfer catalyst were investigated by orthogonal experiment.The optimum reaction conditions were obtained as follows:B/D=1.1,P/D=0.10%,t=6 h,T=50 ℃.The yield of ADPP reached 86.3% under these conditions.Moreover,ADPP was characterized by IR,1H NMR,MS and elemental analysis.