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以三氯氧磷与四甲基脲为原料,六氟磷酸钾为离子交换剂,合成中间体N,N,N’,N’-四甲基氯甲脒六氟磷酸盐(TCFH),将合成的TCFH与1-羟基苯并三氮唑的钾盐(KOBt)反应合成苯并三氮唑-N,N,N’,N’-四甲基脲六氟磷酸盐(HBTU).通过红外光谱、核磁共振波谱以及液相色谱等对产物进行表征.研究了离子交换剂类型、二氯甲烷用量、滴加时间、滴加温度对中间体TCFH收率的影响以及反应时间与转速对HBTU收率的影响.结果表明,以六氟磷酸钾为离子交换剂、二氯甲烷与三氯氧磷体积比为15.6、滴加时间为90 min、滴加温度为25℃时,中间体TCFH收率达60％以上.反应时间、转速对HB-TU产生一定影响,反应15 min时HBTU的总收率可达95％.“,”The intermediate N,N,N’,N’-tetramethyl chloroformamidine hexafluorophosphate (TCFH) is synthesized by using phosphorus oxychloride and tetramethyl urea as raw materials and potassium hexafluorophosphate as ion exchanger.Then benzotriazole-N,N,N’,N’-tetramethyluronium hexafluorophosphate (HBTU) is synthesized through the reaction between TCFH and potassium salt of 1-hydroxybenzotriazole (KOBt).The obtained HBTU is characterized by infrared spectroscopy (FT-IR),nuclear magnetic resonance spectroscopy (1HNMR) and liquid phase chromatography.The effects of variety of ion exchangers,the dosage amount of dichloromethane,dropping time and dropping temperature on the yield of TCFH and the effects of reaction time and rotating speed on the yield of HBTU are both studied.The results show that TCFH yield can exceed 60％ when potassium hexaffuorophosphate is used as ion exchangers,the volume ratio of dichloromethane to phosphorus oxychloride is 15.6:1,dropping time is 90 min and dropping temperature at 25℃.Furthermore,the reaction time and rotational speed both bring some impacts on the yield of HBTU and the overall yield can reach about 95％ with 20 min of reaction time.