1,4-双(2-氰基苯乙烯基)苯的合成工艺改进

以对二甲苯为原料,通过氯化反应,用乌洛托品法水解氯化物合成对苯二甲醛,收率78.4%,含量99.5%。以二甲苯为溶剂,邻腈基苄基氯和亚磷酸三乙酯为原料,通过Abuzov反应合成邻氰基苄基膦酸二乙酯,收率86.5%。邻氰基苄基膦酸二乙酯通过Wittig反应和对苯二甲醛缩合制得1,4-双(2-氰基苯乙烯基)苯,收率84.1%,含量99.5%(HPLC)。

Process improvement on the synthesis of 1,4-bis(o-cyanostyryl) benzene

1,4-Dimethylbenzene was chlorinated by dry Cl2,then the mixed chloride products was hydrolyzed to terephthalaldehyde by hexamethylenetetramine.The purity of the product was 99.5% and the yield is 78.4%.Diethyl o-cyanobenzyl phosphonate was synthesized by the esterification reaction of triethyl phosphatidate and o-cyanobenzyl chloride dissolved in dimethylbenzene,the yield is 86.5%.1,4-bis(o-cyanostyryl)-benzene was synthesized from diethyl o-cyanobenzyl phosphonate and terephthalaldehyde.The purity of the product is 99.5%(HPLC) and the yield is 84.1%.