Study On The Synthetic Technology Of Pyridazinone

3(2H)-Pyridazinone compounds as medicines and pesticides have been developed most quickly and have become a new trend in the present. Especially, 3(2H)-Pyridazinone compounds have taken an important role in the development of pesticides. 3(2H)-Pyridazinone derivatives pesticides are the new pesticide series which come from the reconstruction of insecticidal botany resources after Carbarnate pesticides, Pyrethroid insecticides and Neonicotinoid Insecticides.Aqueous sodium hydroxide solution was added to tert-butylhydrazine hydrochloride and mucochloric acid in the organic solution. After completion of the reaction ,2-tert-butyl-4,5-dichloro-3(2H)-pyridazinone were carried out, the yield was 76%～78%. If adding catalyst acetic acid, heat preservation duration at about 40℃ for 4 h, the yield can be improved. It was about 81%. Using anhydrous sodium acetate replaced sodium hydroxide for the same ratio of mol, the yield also can be increased, and the result is more stability than before. The yield was 82%~84%. The product has been identified by elementary analysis, IR and 1H-NMR. Using anhydrous sodium acetate for industrialization, this method is appropriate to the factory. The results showed that the reaction duration decreased from 12h to 7h, the purity of products increased from 89% to 94%, the yield increased from 78% to 82%, at the same time, the waster water exhausted just half of the past. We got good quality, satisfied yield and less waste water in the industrial production. This method agreed to the environmental protection policy and brought the enterprise satisfied economic & society benefits.Sodium methoxide was added to 2-tert-butyl-4,5-dichloro-3(2H)-pyridazinone and 2-tert-butyl-4-chloro-5-mercapto-3(2H)-pyridazinone in solution, heat preservation duration at about 25℃for 4h. The precipitated solid 2-tert-butyl-5-(4-tert-butylbenzylthio)-4-chloropyridazin-3(2H)-one was filtered off after allowed to cool to low temperature. Using sodium hydroxide, the result was similar with Sodium methoxide. Sodium methoxide as acid acceptor was better than sodium hydroxide after reusing solution. The yield was 87%~89%. The product has been identified by elementary analysis, IR and 1H-NMR.Researched the analytic method of tert-butylhydrazine hydrochloride and2-tert-butyl -4,5- dichloro - 3(2H)- pyridazinone by gas chromatography, when introducing benzaldehyde as derivatization agent, using OV-17 as stationary phase and the method of capillary gas chromatography, tert-butylhydrazine hydrochloride was determined . The quantitative analysis was carried out with internal standard method. The results showed that coefficient of variation was 0.61% and the recovery was 98%～101%. Using dimethyl phthalate as internal standard, OV-225 as stationary phase and chromosorbwaw-DWCS as supporter, 2-tert-butyl-4,5- dichloro-3(2H)- pyridazinone was separated by gas on a stainless packed column of 2m length. 2-tert-butyl-4,5-dichloro-3(2H)-pyridazinone was determined by gas chromatography. The results showed that coefficient of variation was 0.27% and the recovery was 98%～99%.