Study On The Synthesis Of Spirotetramat

Spirotetramat is a new kind of broad-spectrum, high effc ient, low toxic ity, envitonmental friendly pesticides. It has a great application prospects and market prospects because of its high activity,less dosage,strong absorption, wide pesticidal spectrum characteristics and long duration, for people, animals and environment safety.But at present,the synthesis technical process of spirotetremat is not enough mature and the cost of industrial manufacture is higher.Therefor it has very important signficance to find a mature synthes is technology route to reduce the production cost of spirotetramat and improve the yield of the synthesis process. In view of this, this paper based on a large number of literature investigation and research work, the synthes is process of spirotetramat was optimized,the studies in this are summarized as follows:1. 2,5-Dimethylphenylacetic acid was synthesized with para-xylene by chloromrthylation,cyano and acid hydrolysis. The optimized process has some advantagess of mild reaction, high yield, simple operation and less waste, so it is suitab le for industrial production.2. 4-Methoxy cyclohexanone was synthesized with hydroquinone by catalytic hydrogenation, oxidation and methylation.The optimized process is not high requirements on the reaction conditions, and the hydrogenation catalyst Raney nickel can be used repeatedly, the effect of the selective oxidation of sodium bromat is good, so it is suitable for industrial production and has strong market competitiveness.3. Cis-1-amino-4-methoxy cyclohexanecarboxylic acid was synthesized with 4-methoxy cyclohexanone by Bucherer-berg’s reaction and alkaline hydrolysis. In this process,although the yield is not high, but the cis-product content is most and the separation process is reduced and the after is simplified.4. Spirotetramat was synthesized with cis-1-amino-4-methoxy cyclohexyl ac id by esterification, condensation, dickman condensation and substitution reaction, the purity was 96.7%, the total was 16.7%. The cis intermediate can be transformed completely at the optimized process.LC-MS, 1H NMR confirmed that the product was spirotetramat. The production cost, simple operation and maximum yield was explored, which laid a foundation for the future of spirotetramat industrialization.