摘要
以邻甲氧基苯甲醛(OMD)为原料,与丙酮进行Claisen-Schmidt缩合反应形成中间体邻甲氧基苄叉丙酮(OMT),OMT再与NaClO发生卤仿反应得到邻甲氧基肉桂酸(OMA)。优选的工艺条件是:缩合反应中丙酮与OMD的物质的量之比为2.5,反应温度为20~30℃,反应时间为6h;卤仿反应温度为20~30℃,反应时间为8h。经φ=30%乙醇水溶液重结晶后,OMA的总收率按OMD计为81%,气相色谱测得OMA纯度为99.2%。
o-Methoxycinnamic acid (OMA) was prepared by Claisen-Schmidt condensation of o-methoxybenzaldehyde(()MD) with acetone and then by Lieben haloform reaction of the intermediate o methoxybenzalacetone(OMT) with NaClO. Acetone and OMD were condensed with a molar ratio of 2.5at 20-30℃ for 6 h 8 h to obtain OMA purity 99.2G). to obtain crude OMT, which was used directly in haloform reaction at with a total yield of 81% after recrystallization from φ=30% ethanol 20 30 ℃ for solution (GC purity 99.2G).
出处
《华东理工大学学报(自然科学版)》
CAS
CSCD
北大核心
2014年第1期70-73,共4页
Journal of East China University of Science and Technology