甲基环戊二烯基水杨酸钛(Ⅳ)配合物的合成与表征

采用水相法和两相法用二氯二甲茂钛与相应的水杨酸反应合成了 6个配合物 :二甲基环戊二烯基水杨酸钛 ( ) ,二甲基环戊二烯基二水杨酸钛 ( ) ,二甲基环戊二烯基 5 -硝基水杨酸钛 ( ) ,二甲基环戊二烯基二 5 -硝基水杨酸钛 ( ) ,二甲基环戊二烯基 3 ,5 -二硝基水杨酸钛 ( ) ,二甲基环戊二烯基硫代水杨酸钛( ) .对这些化合物进行了元素分析 ,测定了熔点 ,讨论了它们的红外光谱和核磁共振谱 .

水相法合成二氯二甲茂钛与水杨酸类配合物

The complexes of dimethylcyclopentadienyl dichlorotitanium(Ⅳ)and salicytic acid,sulfhydryl salicylic acid,5-nitrosalicylic acid,3,5-dinitro salicylic acid have been prepared in aqueous-phase.The structures have been determined by elemental analysis,IR and 1HNMR spectra. It’s approved that (MeCp) 2TiCl 2-acetylacetone complex reacts with sodium of salicylic acid or substituted derivatives in aqueous-phase,and the results depend on the pH of salicylate solution,concentration and temperature.The best condition of the preparation of dimethylcyclopentadienyl salicylatotitanium(Ⅳ)complexes is that:the molar ration of (MeCp) 2TiCl 2 and substituted salicylic acid is 1:1;the pH being controlled in 6 0-7 5.The disalicylato derivatives of dimethylcyclopentadienyl titanium(Ⅳ)are whereby where by (MeCp) 2TiCl 2 and substituted salicylic acid are close in the molar ratio of 1 to 2,and the pH is 3.5-4.5.In all the preparations,the temperature is at 0℃ and the molar concentration of substituted salicylic acid is 0.04 mol/L.The mechanism of the reaction was also discussed.

甲基环戊二烯的合成研究

以环戊二烯(CPD)、金属钠和一氯甲烷为原料合成甲基环戊二烯,包括制备环戊二烯钠和环戊二烯钠甲基化两步反应。结果表明,反应温度及环戊二烯与钠的摩尔比对甲基环戊二烯的收率影响显著。双环戊二烯的最佳解聚温度为250℃,对于CPD与钠的反应,反应初期温度应控制在较低的温度,以减少CPD二聚反应;反应后期可将温度升高至28℃,以加快CPD与钠的反应速率。最佳的CPD与钠摩尔比为2.2,此时甲基环戊二烯的收率达86%。