1.Synthetic Study About An Ultra-high Effect, Low-toxicity, And Wide-spectrum Herbicide--Bispyribac-sodium 2.Synthesis And Functions Of Noncyclic Ligands Having Plural Phenolic Hydroxyl Groups

Based on extensive study of domestic and foreign journals in the field of herbicide, the history, current status, and development of three kinds of pesticides have been given in the first part of the dissertation. The industrial situation about herbicide in China has been introduced as well as the research and development of the herbicides aiming at high effect and classification of the inhibitors to ALS (Acetolactate Synthase). Moreover, the synthetic routes and methods, acting mechanism, and toxicity about pyrimidinylether herbicides have been described, especially, the physical and chemical properties, toxicity, reaction mechanism, and application about the world novel herbicide-Bispyribac-sodium( or Nominee) on rice have been summarized in detail.This dissertation is particularly focused on studying, innovating, and optimizing of the synthesis of Bispyribac-sodium, a kind of herbicide with high effect on rice and wheat against barnyard grass, green foxtail, and other weeds. The technical material (TC) and its 10% aqueous suspension concentrate (SC) of Bispyribac-sodium were prepared via eight steps, including cycloamination (consisting ammonolysis of ester, aromatization, and salify), methylation, chlorination, methoxylation, oxidation and condensation, and so on, using thiourea, diethyl malonate and sodium methanol as main starting materials. 4,6-dihydroxyl-2-methythio pyrimidine was successfully synthesized by using water instead of 48% sodium hydroxide (NaOH) as reaction solvent. This innovation leds to a great cutting down on amounts of acid and NaOH, more economic, and decrease of pollution. Due to its low melt point and high sensitivity to moisture, 4,6-dichloro-2-methylthio pyrimidine is commonly regarded as a difficult point for dry. In our research, this problem was economically solved, through extracting the product from reaction aqueous with organic solvent. The separation of 4,6-dimethoxy-2-methylthio pyrimidine from inorganic salt and improvement of yield benefited from selecting two kinds of solvents in this methoxylation . Contributed to continuous process of chlorination, methoxylation, and oxidation, not only problems depicted above have been solved, but also the overallyield has been increased by 10% in the three steps. Additionally, the safely synthetic manner of Bispyribac-sodium as well as improvement of yield and reduction of cost by utilizing sodium hydroxide (NaOH) and toluene^HsCHa) replace of sodium hydride (NaH) and tetrahydrofuran (THF) have been obtained. As a result of these innovations, TC and 10% SC of Bispyribac-sodium are being produced in a relatively large scale at some pesticide companies.The final product was characterized by NMR, 1R, UV, and MS spectrum and was proved to be consistent with the structure of the target product.It is worthy to notice that this project has passed the authentication in Zhejiang province, and experts commended accordantly that this achievement reached international advanced level.