He Xiao-xiao
2010
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Journal
Journal of Zhejiang University of Technology
Abstract
An improved process was developed for the synthesis of 4-methyl-2-hydrazinobenothiazole.4-methyl-2-aminobenzothiazole hydrochloride(AMBT·HCl) was synthesized by N-(2-methylphenyl)thiourea and chlorine.4-methyl-2-hydrazinobenothiazole was synthesized by substitution reaction with AMBT and AMBT·HCl as raw materials and ethylene glycol as solvent.The target compound and key intermediate were separated and characterized by gas chromatography(GC),infrared spectrum(IR),nuclear magnetic resonance(NMR).The yield of the target compound can be reached 90.3%(purity of 98.2%).The factors of reaction include the confirmation of reagent,feed molar ratio,solvent,quantity reaction time and reaction temperature.The preferred reaction conditions include that taking chlorine instead of SOCl2 or KBr,the molecular ratio between AMBT and hydrazine hydrate is 1∶6.5,glycol 15 mL,the reaction period is seven hours and the reaction temperature is 115 ℃.The advantages of synthetic route proposed are easy operation,mild reaction condition,high yield and suitable for industrialization.