Studies On The Synthetic Process Of Flubendiamide' Intermediates

Flubendiamide is an insect pesticide of Ryanodine (muscle) receptor activator. The pesticide has a novel structure and mechanism. Flubendiamide can release excessive calcium ions in insects, leading to the insect death. Therefore,the safety of non-target objects, and does not cross resistance to existing insecticides, Flubendiamide is a new promising insecticide.Based on the consulting of the literatures about insecticides ,the domestic and foreign the current word pesticides were summarized. The discovery and the recent development of anthranilic diamides were described. This reported introduces Flubendiamide'history and toxicity, mechanism and application activity.This reported preparation about Flubendiamide'intermediates were also introduced in detail .Based on the related literatures, several synthesis routes of Flubendiamide were evaluated in this paper, therefore an reasonable synthesis of Flubendiamide were explored, including Friedel acylation and oxidation reactions start with 4 - heptafluoro isopropyl aniline, 1,1- dimethyl -2- methylthio-ethylamine, 3 - Iodine phthalate. In this report, the process development of Flubendiamide'intermediates was studied and detailed study on each reaction and the post treatment method were made and optimal condition of each reaction were gotten. During preparing 2 - methyl-4 - heptafluoro isopropyl aniline ( MFA), we found it easy to get raw materials benzylamine sevoflurane and isopropyl iodide as raw material, through free radical reaction, synthesized MFA, the total yield of 90% ,content of 95.0%. And also the molar ratio, solvents, temperature and phase-transfer catalyst were also discussed in the preparing of MFA.During preparing 1,1 - dimethyl -2-- methylthio-ethylamine (VI), we designed 2– amino– 2– methyl– 1 - propanol as material, through reacting with sulfation, and then with methyl mercaptan sodium reaction, the total yield 83.0%, 92.5% more than content. In this reaction of toluene to do with dehydration, effects of sulfuric acid concentration, changes in influencing factors such as feeding mode, effectively reducing the amount of sulfuric acid concentration and reduce the cost and simplify operations, improve the safety factor.During preparing 3 - Iodine phthalate we designed 2,3-dimethyl aniline as material, through diazotization, oxidation, the total yield of 52.5% content of 95.0% above. The ultimate product and its important intermediates were confirmed by 1H NMR,LC-MS.