摘要
以对氯甲苯(PCT)和金属镁为原料,碘引发剂下进行Grignard反应制备对甲基苯基氯化镁,然后与邻氯苯腈(OCBN)在过渡金属化合物催化不对称偶联反应制备2-氰基-4′-甲基联苯(OTBN)。结果表明:以过渡金属MnCl 2为催化剂,四氢呋喃(THF)和2-甲基四氢呋喃(MeTHF)混合溶剂下,可有效调控不对称偶联反应中产物的分布和区域选择。该合成路线具有催化效果好、溶剂回收率高、环境友好、成本低廉、操作简便等特点,易于实现工业化生产。
p-Methylphenylmagnesium chloride was synthesized by Grignard reaction under iodine initiator,p-chlorotoluene(PCT)and metal magnesium using as raw materials,then 2-cyano-4′-methylbiphenyl(OTBN)was prepared by asymmetric coupling reaction with o-chlorobenzonitrile(OCBN),transition metal compound over catalyst.The results showed that the product distribution and region selection in asymmetric coupling reaction could be effectively controlled by using transition metal MnCl 2 as catalyst,and under conditions of mixed solvent of tetrahydrofuran(THF)and 2-methyltetrahydrofuran(MeTHF).The synthesis route had significant advantages,including good catalytic effect,high solvent recovery,friendly environmental,low cost and simple operation,which was convenient for industrialization.
作者
刘建武
严生虎
张跃
LIU Jian-wu;YAN Sheng-hu;ZHANG Yue(School of Pharmaceutical and Life Sciences,Changzhou University,Changzhou 213164,China;Continuous Flow Engineering Laboratory of National Petroleum and Chemical Industry,Changzhou 213164,China)
出处
《化学研究与应用》
CAS
CSCD
北大核心
2021年第1期156-161,共6页
Chemical Research and Application
基金
江苏省产学研前瞻性联合研究项目(BY2014037-19)资助。