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以茚(Indene)和双环戊二烯(DCPD)为原料,通过Diels-Alder双烯加成反应制备非晶型环烯烃共聚物(COC)光学材料单体1,4-亚甲基-1,4,4a,9a-四氢芴(Ind-CPD)。考察了茚(Indene)和双环戊二烯(DCPD)物质的量比、反应温度、压力和时间对加成反应的影响,确定较佳的工艺条件:茚与双环戊二烯的物质的量比为2.2∶1,反应时间3h,反应温度180℃,反应压力0.2MPa。在此条件下,Ind-CPD产品收率为80.5%(以原料茚计),纯度为99.5%[面积归一化法(GC)],三环戊二烯(TCPD)和寡聚物的生成得到有效控制。产物结构经过1 H NMR和MS表征。
Indole (Indene) and dicyclopentadiene (DCPD) were used as raw materials to prepare 1,4-methylene-1, an amorphous monomer of cycloolefin copolymer (COC) 4,4a, 9a-tetrahydro fluorene (Ind-CPD). The effects of the ratio of indene and DCPD, the reaction temperature, pressure and time on the addition reaction were investigated. The optimum process conditions were as follows: the ratio of indene to dicyclopentadiene 2.2: 1, reaction time 3h, reaction temperature 180 ℃, reaction pressure 0.2MPa. Under these conditions, the yield of Ind-CPD product was 80.5% (as raw material indene) with a purity of 99.5% [area normalization (GC)], tricyclopentadiene (TCPD) and oligomer formation Get effective control. The product structure was characterized by 1 H NMR and MS.