Shi Gang
2011
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Journal
Journal of University of Jinan
Abstract
Improvement in the synthesis of 2-(5-Amino-1,2,4-thiadiazol-3-yl)-2-(z)-methoxyimino acetic acide 2-benzo-thiazolyl thioester was studied in the condition of mixed solvent and substitution of triethyl phosphate by triphenylphosphine as condensation catalyst.By orthogonal test,the influence of solvents,temperature and time on the yield and quality of active ester was researched.An improved procedure is established:when n(2-(5-Amino-1,2,4-thiadiazol-3-yl)-2-(z)-methoxyimino acetic acide):n(DM)∶n(triethyl phosphate) equals 1∶1.1∶1.2,V(dichloromethane)∶V(acetonitrile)=1∶1,the product is obtained through four hours at 25℃ with a yield of 94.8%.The measured purity of the product is 99.2%.