The Synthesis Of Nitrogen Heterocyclics Compounds And 4-hydroxycoumarin Green Production Technology

Nitrogen heterocyclic compounds such as 1-phenyl-1H-pyrazole-4-carboxylic acid and oxygen heterocyclic compounds such as 4-hydroxycoumarin are important intermediates in the pharmaceutical, pesticide, dye, catalyst. So they have a very wide range of applications. In recent years, many of studies had found that 4-hydroxycoumarin and its derivatives are an important class of biological anti-HIV, anticoagulant activity of drug intermediates. With the functions in sterilization, insecticidal, anticoagulant, they can be used for anti-tumor, anti-oxidation, anti-radiation, subdue blood pressure. And they also have excellent optical properties. They are good fluorescent brighteners, laser dyes, fluorescent probe and nonlinear optical materials. In addition, it is also a kind of spice, they have attracted considerable interest because of these important characteristics.In this paper, 1-phenyl-1H-pyrazole-4-carboxylic acid was synthesized through three steps from the beginning of phenylhydrazine; 4-methyl-2-(methylamino)thiazole-5- sulfonamide was synthesized through five steps from the beginning of chloroacetone; ethyl 2-p-tolylthiazole-4-carboxylate was synthesized through two steps from the beginning of methyl benzonitrile. They are characterized by NMR. And we also investigated the effects taked by time and temperature. Begin with Zinc tetrafluoroborate, 4,4 '- dipyridyl, terephthalic acid, we synthedized poly[[[tetraaquazinc(II)]-4,4'-bipyridine-N,N']benzene-1,4-dicarboxylate] with the method of hydrothermal. And it was characterized by single-crystal X-ray diffraction.In this paper, we found a new method in synthesis of 4-hydroxycoumarin with solvent-free. The products of each step are analyzed and characterized by GC-MS, NMR, HPLC.We designed orthogonal experiment to test the effects which had by temperature, time and proportion of material on the yield in each step. Finally, we ensure the optimization reaction conditions. On this basis, we carried experiments at the scale of 20 Kg and 50 Kg. After the experiments, we have a technological design on the production of 4-hydroxycoumain, and preliminary assessment of technical and economic analysis. At last, we proposed management ideas on dealing with wastes. This technological design provided consultations to industrial production.