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以4-硝基苯酚为原料,在无水K2CO3和乙腈的作用下,与氯乙酸乙酯反应制得4-硝基苯氧乙酸乙酯,收率90.1%;再以无水乙醇为溶剂,于80-85℃,与w(水合肼)=85%的反应3 h,制得4-硝基苯氧乙酰肼,收率79.7%;然后该化合物以吡啶作缚酸剂,三氯氧磷作酰氯化试剂,室温条件下与苯甲酸反应,制得N,N′-二酰基肼,收率90.6%;最后N,N′-二酰基肼在三氯氧磷作用下,脱水环化合成了最终产物2-(4-硝基苯氧甲基)-5-苯基-1,3,4-噁二唑,收率88.2%.通过IR,1H NMR,13C NMR对上述化合物的结构进行了表征.
Using 4-nitrophenol as raw material, 4-nitrophenoxyacetic acid ethyl ester was obtained by reaction with ethyl chloroacetate under the action of anhydrous K2CO3 and acetonitrile, the yield was 90.1%; then with anhydrous ethanol as solvent, At 80-85 ℃, reaction with w (hydrazine hydrate) = 85% for 3 h, 4-nitrophenoxyacetohydrazide was obtained in a yield of 79.7%. Then the compound was treated with pyridine as acid-binding agent, phosphorus oxychloride As acyl chloride reagent, reacted with benzoic acid at room temperature to obtain N, N’-diacylhydrazine in a yield of 90.6%. Finally, N, N’-diacylhydrazine was dehydrated and cyclized under phosphorus oxychloride The final product 2- (4-nitrophenoxymethyl) -5-phenyl-1,3,4-oxadiazole was obtained in a yield of 88.2%. The structure of the above compound was characterized by IR, 1H NMR and 13C NMR Characterization.