Research On Visible Light Induced C-H/N-H Bond Functionalization Reaction And Optimization Of Synthesis Process Of Dithiophosphate

C-H/N-H bond functionalization has received a lot of attention in recent years,which has greatly facilitated the synthesis of drug molecules,organic dyes and alkaloids.As people become more environmentally conscious,they begin to look for green,efficient and environmentally friendly ways to achieve such reactions.As a clean energy source,the visible light-induced reaction has the advantages of simple operation,wide range of sources and mild reaction conditions,which can well achieve the goal of"green chemistry".Based on this,we have selected simple and readily available nitrogen-containing compounds and sulfonamides to investigate the visible light-induced functionalization of C-H/N-H bonds,and finally achieve the construction of sulfonamides and sulfonamides with higher atomic and step economy.Organophosphorus flame retardants are the most widely used flame retardants,including dithiophosphate flame retardant synthesized from neopentanediol,which is widely used in the field of adhesive fiber.However,the traditional acid binder is easy to cause environmental pollution and human safety,so it is important to study the synthesis method of environment-friendly flame retardant.In this paper,the synthesis of dithiophosphate is optimized to reduce environmental pollution and facilitate industrial production.The details are as follows:1.Using p-toluenesulfonazide and N,N,N’,N’-tetramethylethylenediamine as substrates,the optimal reaction conditions were obtained by optimizing the light source,solvent and concentration,functionalization of C-H bonds without catalysts or additives,and the applicability of substrates was investigated.This method is green and environmental friendly,and a new method for synthesis of sulfonamidines is realized without transition metal catalysis.Structure characterization and analysis of ¹H NMR and ¹³C NMR were performed on the target compounds.2.N-H bond functionalization was achieved in visible-light conditions using p-toluene sulfonyl diazide and N-dimethylethylamine compounds as substrates.A novel method for the gentle synthesis of sulfonamide compounds was developed without photocatalysts or additives.Studies on substrate suitability have found that multiple functional groups are resistant to this response,with yields ranging from moderate to above.Structure characterization and analysis of ¹H NMR and ¹³C NMR were performed on the target compounds.3.A series of screening and optimization of the solvent,reactant equivalents and catalyst equivalents for the synthesis of flame retardant dithiophosphate were carried out.The innovative use of sodium hydroxide as binding acid for synthesis of intermediates and dithiophosphate determined the suitable synthetic route for industrial production,and the reaction could be completed within 10 h,which reduced the pollution to the environment and greatly reduced the cost,and the post-treatment was simple and less polluting.