摘要
以己二酸二甲酯(DMA)为起始原料,经迪克曼缩合、羟醛缩合反应制得3-(4-氯苄基)-2-氧代环戊烷羧酸甲酯。研究了工艺条件对反应的影响。实验表明,制备2-氧代环戊烷羧酸甲酯的适宜工艺条件为:反应温度90℃,反应时间4 h,DMA和甲醇钠的摩尔比为1∶1.05,收率达82.6%;3-(4-氯苄基)-2-氧代环戊烷羧酸甲酯的适宜工艺条件:反应温度90℃,反应时间15 h,2-氧代环戊烷羧酸甲酯和甲醇钠的摩尔比为1∶2.5,收率达89%,熔点为129.9～130.3℃。
Methyl 3-（ 4-chlorobenzylidene）-2-oxocyclopentanecarboxylate was prepared via Dieckmann condensation and aldol reaction using dimethyl adipate as raw material. The effect of reaction conditions on reaction was studied. The experiment showed that the yield of methyl 2-cyclopentanoneearboxylate can be up to 82.6% under reaction temperature 90 ℃ ,reaction time 4 h and the molar ratio of dimethyl adi- pate to sodium methanolate being 1：1.05 ;the yield of methyl 3-（4-chlorobenzylidene）-2-oxocyclopentan- eearboxylate can be up to 89% under the following conditions：reaction temperature 90 ℃, reaction time 15 h and the molar ratio of methyl 2-cyclopentanonecarboxylate to sodium methylate being 1 ： 2.5, the structure of the product was characterized by 1H NMR with the melting point of 129.9 - 130.3 ℃.
出处
《应用化工》
CAS
CSCD
2013年第5期907-909,938,共4页
Applied Chemical Industry
