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以氯化亚铜(CuCl)为催化剂,亚硝酸叔丁酯(t-BuONO)为重氮化试剂,在溶剂乙腈或丁酮中,1-(5-氨基-2-氟-4-氯苯基)-3-甲基-4-二氟甲基-1H-1,2,4-三唑啉-5-酮(TZLO-A)经重氮化和Meerwein芳基化“一锅法”制备得到目标化合物唑草酮,产物经1HNMR、13CNMR和MS表征。合成条件经实验优化,确定了最佳反应条件:n(TZLO-A)∶n(氯化亚铜)∶n(丙烯酸乙酯)∶n(亚硝酸叔丁酯)=1∶(0.6~0.7)∶13.7∶1.5,盐酸(HCl)和亚硝酸叔丁酯滴加时间分别为20 min和150 min,产品收率达到了92.9%,HPLC色谱含量为92%。
Using cuprous chloride (CuCl) as catalyst and tert-butyl nitrite (t-BuONO) as reagent for diazotization, 1- (5-amino-2-fluoro-4-chlorobenzene Yl) -3-methyl-4-difluoromethyl-1H-1,2,4-triazolin-5-one (TZLO-A) diazotized and Meerwein arylated “ ”Preparation of the target compound oxacillin, the product by 1HNMR, 13CNMR and MS characterization. The optimal reaction conditions were determined by the optimized conditions of synthesis: n (TZLO-A): n (cuprous chloride): n (ethylacrylate): n ): 13.7: 1.5. The dropping time of hydrochloric acid (HCl) and t-butyl nitrite were 20 min and 150 min, respectively. The yield of product reached 92.9% and the content of HPLC was 92%.