乙炔双羰基化催化合成丁(烯)二酸二丁酯  

Synthesis of Esters of Succinic Acid by Acetylene Dicarbonylation

作　　者：赵简 孙腾[1] 李建国[1] 杨先贵[1] 王公应[1] HAO Jian;SUN Teng;LI Jian-guo;YANG Xian-gui;WANG Gong-ying(Chengdu Institute of Organic Chemistry,Chinese Academy of Sciences,Chengdu 610041,Sichuan,China;University of Chinese Academy of Sciences,Beijing 100049,China)

机构地区：[1]中国科学院成都有机化学研究所,四川成都610041 [2]中国科学院大学,北京100049

出　　处：《精细化工》2019年第6期1138-1143,共6页Fine Chemicals

基　　金：四川省科技计划项目(2018FZ0082,2016GZ0228)~~

摘　　要：以乙炔(C2H2)、CO和正丁醇为原料,采用PdBr2为主催化剂,在常压、55℃条件下,双羰基化一步合成丁(烯)二酸丁酯。考察了催化剂用量、助剂种类及用量、溶剂种类、反应温度和反应时间对丁(烯)二酸二丁酯收率的影响。结果表明,在Pd Br2用量0.04g,n(PdBr2)∶n(LiBr)=1∶8,甲基磺酸0.1 mL,30 mL乙腈为溶剂,n(C2H2)∶n(CO)=1∶2,101 kPa,55℃,反应3 h的反应条件下,丁(烯)二酸二丁酯的收率达到76.11%。Esters of succinic acid were synthesized by dicarbonylation of acetylene and carbon monoxide in the presence of n-butanol using PdBr2 as main catalyst under normal pressure and 55 ℃ conditions. The effects of the amount of catalyst, type and amount of auxiliaries, type of solvent, reaction temperature and reaction time on the yield of the products(dibutyl succinate, dibutyl maleate and dibutyl fumarate) were investigated. The experimental results showed that the optimal conditions were as follows: amount of PdBr20.04 g, n(PdBr2)∶n(Li Br)=1∶8, methanesulfonic acid 0.1 mL, acetonitrile as solvent 30 mL, n(C2H2)∶n(CO)=1∶2, pressure 101 kPa, reaction temperature 55 ℃ and reaction time 3 h. Under these conditions,the yield of dibutyl succinate, dibutyl maleate and dibutyl fumarate reached 76.11%.

关 键 词：乙炔 羰基化 丁二酸二丁酯 丁烯二酸二丁酯 催化技术 

分 类 号：TQ225.24[化学工程—有机化工]