The Study On The Preparation Process For Lithium Bis(Trifluoromethane Sulfonyl)imide And Kresoxim-methyl

The thesis is divided into two parts.Part I: The study on the preparation process for Lithium bis(trifluoromethane- sulfonyl)imide.Lithium bis(trifluoromethanesulfonyl)imide ((CF3SO2)2NLi) is the first member of bis(trifluoromethanesulfonyl)imide salt of the compound series. In the strong effect of the electron's collaborative participation of trifluoromethyl. Lithium bis- (trifluoro- methanesulfonyl)imide ion in the negative charge on N atoms can be resonantly scattered throughout the O-S-N backbone and a high degree of delocalization, thereby greatly enhancing the stability of ion. On the other hand, two large volume trifluoromethyl steric make such coordination capacity of the ion are highly reduced. It demonstrates the potential power of a strong chemical affinity, high Lewis acidity and high-quality solid surface characteristics.Thus making such material in many fields have a wide range of uses. For example,preparation of lithium ion battery electrolyte, ionic liquid, selective fluorination reagents and environmentally friendly and efficient Lewis acid catalyst.This part of the thesis, two methods were discussed and compared the process for preparation of bis(trifluoromethanesulfonyl)imide lithium. The first method was to use trifluoromethanesulfonate acid as a starting material. First, it reacted with phosphorus pentachloride to obtain trifluoro methanesulfonyl chloride. Under the catalytic action of triethylamine or pyridine. After ammonolysised, trifluoro methanesulfonyl chloride, Again reacting trifluoroacetic methanesulfonyl chloride, obtained bis(trifluoromethanesulfonyl)imide triethylamine or pyridine salt. It was under the effect of sodium hydroxide obtained bis (trifluoromethanesulfonyl)imide sodium salt. After acidulating of sulfuric acid obtained the bis- (trifluoromethane- sulfonyl)imide. Finally, obtained the final product lithium bis (trifluoromethane- sulfonyl)imide under the action of lithium carbonate. The total yield was about 25%.The second method used trifluoro methanesulfonyl fluoride instead of trifluoro methanesulfonyl chloride as the starting material, taken withthe first method similar to the process. Final yield was about 78%.The latter process is simple, low cost, low pollution, high yield and good quality. At the same time, by-product ammonium fluoride, sodium fluoride and sodium. It is suitable for industrial production, which has important application value. This method is suitable for industrial production, which has important application value.Partâ…¡: The study on the preparation process for kresoxim-methyl.Kresoxim-methyl was prepared by BASF which followed a nature-based mushroom biomimetic synthesis of natural products with new modes of action of a disinfectant.The preparation of the product name for"Stroby", It is an excellent new fungicide. It has four characteristics. First, it has high activity, at the same time it has good protection and treatment. Second, there is a long period could be kept. And no cross-resistance to other commonly fungicides. Third it has a broad spectrum bactericidal, and it imperfect fungi, Ascomycetes,Basidiomycetes, Oomycetes and other fungi caused by a variety of diseases has good activity. Fourth, it has low toxicity and high efficiency, low-residue, highly selective, It makes crops, livestock, non-target organisms and environmental safety.This paper had discussed a variety of synthesis methods. First, we selected the tert-butyl toluene as the starting material. Through two Friedel-crafts reaction, and then get keto ester. However, duing to the lower yield of the method had to be abandoned. Finally,we selected o-bromo toluene as the starting material to obtain Grignard reagent, Grignard reagents and monomethyl oxalyl chloride was conjugated reaction and obtained keto esters. And then condensation with the methoxamine hydrochloride obtained important intermediate oxime. It is then brominated by NBS, then it reacted with o-cresol sodium and obtained (Z), (E) - kresoxim mixture. This mixture dissolved in dry methanol, under hydrogen chloride obtained by the (E) - kresoxim, the total yield more than 30%. The process is simple and readily available raw materials, low cost, low pollution, high yield, good quality, it is worth to promote industrialization.The two parts of the intermediate and final products were characterized by NMR, IR and elemental analysis.