Of N, Of N-(r <sub> 1 </ Sub>, R <sub> 2 </ Sub>) -3 - Amino -1,2 - Propylene Glycol Compounds In Catalytic Synthesis Of Research

N,N-(R1,R2)-3-amine-1,2-propanediol is a series of important pharmic intermediats, which is used in medicine and pesticide producing industry extensively. Take 3-amino-1,2-propanediol for example, it is a very basilic intermediat of synthesizing non-ionic x-ray contrast agents Iohexol and Ioversol. Its purity is a direct influencing factor to the quality of Iohexol and Ioversol, and its producing cost influences the output costs of Iohexol and Ioversol. Other N,N-(R1,R2)-3-amine-1,2-propanediol also is a kind of usual chemical raw material, and it is extensively used in drug synthesis, polymer materials producing, polyurethane industy. Recently, It is reported that such polyhydroxy amines as a linker had a high research and application value in synthetic nucleotide research. Nowadays, at home, there are many problems in synthesizing the compounds, such as long reaction time, low yield, poor aftertreatment course, and the purity could not meet the demands of downstream manufacturers.During our research, we synthesized 3-amino-1,2-propanediol using 3-chloro-1,2-propanediol as the material, and studied on the catalytic synthesis process, the mechanism of reaction. First of all, we screened and prepared a complex catalyst which could raise the yield of 3-amino-1,2-propanediol and optimized the process conditions of synthesis. In aftertreatment process, the crude product went through the process of expulsing excess ammonia, regulating pH, vacuum distilling water, dissolving target product and depigmentation, filtration, evaporating solvent, vacuum molecular distillation respectively, then got the high pure 3-amine-1,2-propanediol. The whole set of synthesis technology shortened the reaction time, and raised the yield of target products, in the process of synthesis reaction, it had a mild reaction condition and it was no need to separate the intermediate product, so it achieved synthesis in one pot.Based on the job above, according to its synthesis mechanism, on condition that the similar synthesis technology was usded, we tried to synthesize other N,N-(R1,R2)-3-amine-1,2-propane-diol by the action of the complex catalyst which we used in synthesizing 3-amine-1,2-propanediol. We synthesized N-methyl-3-amine-1,2-diol, N,N-dimethyl-3-amine-1,2-diol, N,N-diethyl-3-amine-1,2-propanediol and tried to synthesize N-phenyl-3-amine-1,2-propanediol, N-pmethylpheny 1-3-amine-1,2-propanediol,3-pyrrolyl-1,2-propanediol. Thereinto, the synthesis reactions of N,N-diethyl-3-amine-1,2-propanediol, N-phenyl-3-amine-1,2-propanediol, N-pmethy-lphenyl-3-amine-11,2-propanediol and 3-pyrrolyl-1,2-propanediol have not been reported by related literatures, and the others compounds'yield all raised remarkably compared with the related literatures.The target compounds were investigated by FT-IR,1H NMR,13C NMR and MS. We corroborated the chemical structure of the compounds:3-amine-1,2-propanediol, N-methyl-3-amine-1,2-propanediol, N,N-dimethyl-3-amine-1,2-propanediol, N,N-die-thyl-3-amine-1,2-propanediol. In the groping process of synthesizing N-phenyl-3-am-ine-1,2-propanediol, N-pmethylphenyl-3-amine-1,2-propanediol,3-pyrrolyl-1,2-prop-anediol, we also did some necessary tests and got the related spectrum data.Based on above research, we preliminary designed a pilot synthetic technical process of 3-amine-1,2-propanediol and it is a 200 t/year pilot technical scheme. We designed the flow chart and did the material balance of this pilot process. And we leaded an Intermal-recycling Film Molecular distillator into the process of product purification and the equipement could raise the efficiency of distillation and the purity of products. Then, the quality of these products can meet the demands of downstream producer.The catalytic synthesis method and pilot technical process which described in the thesis can offer the thread of synthesizing other similar compounds and the process of lab to industrialization. If details of the research are ameliorated under the future research, it will have a bright applied prospect and bring immense economic benefits.