The Optimization Of The Synthesis Process Of Sabiphos

Anilofos(Drug Code:83301)is a kind of thiophosphate herbicide which is mainly applied in controlling the annual grasses and family cyperaceaes existed in rice field.In this paper,the synthetic technology of anilofos was researched to obtain a green high-yield,high-purity,low-three wastes and low-cost synthetic route.First,the synthetic route of anilofos was determined from 4-chloro-N-isopropylaniline and phosphorus pentasulfide separately via chloride acetylation,phosphorylation and condensation.The total yield was up to 91%,and the purity was up to 97%.There was no threewastes emission during the chloride acetylation.And the water was used as solvent and the anilofos was detached from water during the condensation.Besides,the environment pollution was improved by recycling the mother liquid to reduce wasterwater volume.At last,the green synthetic technology was achieved.In addition,based on the laboratory test,the anilofos was prepared in enlarging production,and the productive task of kilogram-scale was completed finally.It confirmed that the synthetic route can meet the need of commercial production.The structures of intermediate and anilofos were confirmed by H-NMR and 13C-NMR.Finally,the impurities of anilofos and CCPA were isolated by column chromatography,TLC separation and HPLC separation,and their structures were determined by ’H-NMR,13C-NMR,GC-MS,LC-MS and MALDI-TOF-MS.According to their structures,the sources were analyzed to lay the foundation of improving anilofos purity.