2-丁二酸单乙酯酰基-9,9-双甲氧甲基芴的合成  

SYNTHESIS OF 2-MONOETHYL SUCCINYL-9,9-BIS(METHOXYMETHYL) FLUORENE

作　　者：王华[1] 宋磊 杨勇[2] 方宏 王涛[1] 王世华 丁伟[3] 

机构地区：[1]中国石油大庆化工研究中心,黑龙江大庆163714 [2]大庆石化公司实业总公司,黑龙江大庆163714 [3]大庆石油学院,黑龙江大庆163318

出　　处：《精细石油化工》2009年第1期59-63,共5页Speciality Petrochemicals

摘　　要：通过分子设计确定了一种新型醚酯类内给电子体的合成路线,即以芴、多聚甲醛和乙醇钠等为主要原料,经过醚化、酯化和Friedel-Crafts酰基化等反应合成了9,9双羟甲基芴(BHMF)、9,9双甲氧甲基芴(BMF)、丁二酸单乙酯和丁二酸单乙酯酰氯(ESC)4种中间体,并最终合成出目的产物2-丁二酸单乙酯酰基9,9-双甲氧甲基芴。确定的最佳反应条件为:n(BMF):n(ESC)=1:1.1,n(BMF):n(无水三氯化铝)=1: 2.2,反应时间为9 h。利用红外光谱、核磁共振氢谱和碳谱对中间体和目的产物的结构进行了表征和分析,特征峰与所设计的分子结构相符合。A novel process for the synthesis of 2-monoethyl succinyl-9,9-bis（methoxymethyl）fluorene was established through molecular design. Four intermediate products were synthesized through etherification, esterification and Frieded-Crafts acylation, with fluorine, paraformaldehyde, sodium ethoxide, etc. as primary raw materials, i. e. , 9,9-bis- （hydromethyl）fluorene, 9,9-bis（methomethyl）fluorene, monoethyl succinate and monoethyl succinyl chloride. The optimum reaction conditions were obtained by orthogonally arranged experiments： molar ratio of 9,9-bis（methomethyl）fluorene to monoethyl succinate 1 ： 1.1, molar ratio of 9,9-bis- （methomethyl）fluorene to AlCl3 （no water） 1 ： 2.2 and reaction time 9 h. The structures of the intermediates and the final product were characterized by FT-IR, 1H-NMR and ^13C NMR. It was found that the characteristic peaks of both the intermediates and the final product are in accord with the initial designed configurations.

关 键 词：丙烯聚合 Ziegler—Natta催化剂 内给电子体 合成 芴 多聚甲醛 乙醇钠 

分 类 号：TQ032[化学工程]