Study On The Synthesis Process Of Cp₂TiCl₂ And The Synthesis Methodology Of Catalyzed Synthesis Of Phthalazinone Compounds

Titanocene dichloride is an organometallic compound with a stable structure,which has a wide range of applications in the fields of biology,medicine and chemical industry.Therefore,this paper optimizes a series of process parameters based on the traditional diethylamine method for the preparation of titanium dichlorocene to make the process more economical and environmentally friendly.Diazaphthalenones are a class of nitrogen-containing heterocyclic compounds with significant biological activity and various biological properties such as anticancer,anti-inflammatory,antibacterial,antioxidant and anti-neurodegenerative,etc.The synthesis methods of diazaphthalenones reported in the literature have various problems such as harsh reaction conditions,accumulation of heavy metals,low yields,and not easy to be scaled up,thus exploring simple,efficient and economically feasible synthesis methods.Therefore,the investigation of simple,efficient and economically feasible synthesis methods is still the focus of research on diazanonaphthalenes.A study on the synthesis process of titanium dichlorodicarbide.Firstly,cyclopentadiene monomer was obtained from dicyclopentadiene dimer by distillation.Then,cyclopentadiene monomer and titanium tetrachloride were used as raw materials and diethylamine was used as base.By optimizing the process parameters such as solvent,temperature,time and molar ratio of raw materials in the process route,the optimal process conditions were obtained,resulting in an increase of titanium dichlorodimers yield from 33%to 59%and purity from 90%to 99%.Meanwhile,the reuse of the washing solution greatly reduced the reaction cost and made the post-treatment process more environmentally friendly.On the synthesis of diazaphthalenones,a series of diazaphthalenones were synthesized efficiently using only 1 mol%of the synthesized titanocene dichloride as a precatalyst and ethanol as a mating solvent in cooperation with titanocene dichloride catalyzing o-carboxybenzaldehyde and hydrazine derivatives in 90%?99%yield and98%?99%purity,based on the process optimization of titanocene dichloride.The catalyst dosage,reaction temperature and reaction time in the reaction system were optimized,and the catalytic mechanism of ethanol synergized with titanium dichlorodichloride was explored by the follow-up monitoring of ¹H NMR and ¹³C NMR and the analysis of solvent effect.The amplification experiments and the recycling of catalytic intermediates showed that the method is industrially and environmentally feasible.