新型脱氢松香酰肼基硫脲的研究  

Synthesis of New Hydrazidyl-thiourea Based on Natural Rosin Derivatives

作　　者：王秋萍 黄青则 黄世勇 黄媚 雷福厚 申利群 WANG Qiuping;HUANG Qingze;HUANG Shiyong;HUANG Mei;LEI Fuhou;SHEN Liqun(Guangxi Research Institute of Chemical Industry Co.Ltd.,Nanning 530001,China;College of Chemistry and Chemical Engineering,Guangxi University for Nationalities,Nanning 530006,China)

机构地区：[1]广西化工研究院有限公司,广西南宁530001 [2]广西民族大学化学化工学院,广西南宁530006

出　　处：《化工技术与开发》2019年第11期32-36,共5页Technology & Development of Chemical Industry

摘　　要：以松香改性产品脱氢枞胺为原料,乙醚为溶剂,在-10~40℃下与二硫化碳(CS2)、N,N’-二环己基碳二亚胺(DCC)作用,合成脱氢松香异硫氰酸酯,最高产率为84.1%。然后以对甲苯磺酰氯、苯磺酰氯、水合肼为原料,四氢呋喃为溶剂,在10~15℃下分别合成对甲苯磺酰肼(最高产率91.9%)和苯磺酰肼(最高产率96%)。最后,松香异硫氰酸酯分别与对甲苯磺酰肼、苯磺酰肼反应,乙醇为溶剂,于60~80℃条件下回流搅拌,合成了対甲苯磺酰肼基脱氢枞氨基硫脲和苯磺酰肼基脱氢枞氨基硫脲,最大收率均大于60%。所合成的化合物经红外光谱、核磁共振谱等表征分析,证实是一种未见报道的新化合物。The dehydroabietic isothiocyanate was synthesized from dehydroabietylamine,which reacted with carbon disulfide(CS2)and N,N’-dicyclohexylcarbo-diimide(DCC)using ethyl ether as the solvent at-10~40℃,with the highest yield of 84.1%.Then,two intermediates of toluene sulfonyl hydrazide and benzenesulfonyl hydrazide were synthesized by the reaction of hydrazine hydrate and p-toluene sulfonyl chloride or benzensulfonyl chloride using tetrahydrofuran as the solvent at 10~15℃,with the highest yields of 91.9%and 96%,respectively.Finally,the new hydrazidyl-thiourea of p-toluenesulfonyl hydrazine dehydroabietic aminothiourea and benzenesulfonyl hydrazine dehydroabietic aminothiourea were synthesized by the reaction of dehydroabietic isothiocyanate and toluene sulfonyl hydrazide or benzenesulfonyl hydrazide using ethanol as the solvent at 60~80℃,with the highest yield more than 60%,respectively.Moreover,the compounds were characterized by IR and NMR and the results demonstrated that the final products both were new compounds unreported before.

关 键 词：脱氢枞胺 脱氢松香异硫氰酸酯 对甲苯磺酰肼 苯磺酰肼 硫脲衍生物 

分 类 号：TQ468.4[化学工程—制药化工]