Synthesis And Study On Technology Of 2-imidazolidinone Derivatives And Trifluoroacetic Acid

This paper consists of two parts:the first part is the synthesis and studying on 2-imidazolidine derivatives. The second part is the study on the technology of trifluoroacetic acid.PartⅠ:In this part, the synthesis routine of 2-imidazolidone derivatives were designed from the angle of view of industrialization, and fifteen compounds such as 1-Methanesulfonyl-2-imidazolidinone,3-Chlorocarbonyl-1-methanesulfonyl-2-imidazolidinone,1-Chlorocarbonyl-2-Imidazolidone and so on were synthesized. The molecular structures of fifteen products were characterized by 1HNMR and measuring melting-point, and the compounds obtained was final objective products. A new technology to synthesis of 1-Methanesulfonyl-2-imidazolidinone using methanesulfonic anhydride to replace methanesulfonyl chloride was put forward. This method was of characteristic of high yield, safe operation, the widely sources of raw material, low cost and so on. The effect factors on the new technology were investigated systematically, from the results it was concluded that the optimum technique was: methanesulfonic anhydride:Triethylamine:2-imidazolidinone (mol)=1.25:1.25:1, the reaction temperature was 80℃, reaction time was 6 hours and solvent was benzene or toluene. Under solvent-free condition, 1-(2-Aminoethyl)-2-imidazolidinone was synthesized by cyclization reaction at high temperature. The materials, reaction temperature and reaction time were discussed, and the optimum reaction condition was Diethylenetriamine:Urea (mol)=2:1, at the temperature of 200-210℃and reaction time of 4 hours.PartⅡ:Trifluoroacetic acid was prepared by oxidation reaction from 2,2,2-Trifluoroethanol. The preparation process has advantages of sample apparatus, high product purity and low reaction temperature. The optimum technological condition was determined by systematically studying the effect factors and was that:chromic oxide as oxidant,2,2,2-Trifluoroethanol oxidation=1:1.25, at 80-100℃for 4 hours. Using 30%(mass fraction) sodium hydroxide solution neutralized the reaction solution, trifluoroacetic acid could be obtained with purity higher than 98%, the highest yield was 77%. Study on recycling of trifluoroacetic acid distillation mother liquid,2,2,2-Trifluoroethanol:sulfuric acid (mol)=1:5, the trifluoroacetic acid distillation mother liquid can recycle 3 time without obvious fluctuation.