p-Dimethylaminophenylpentazole(p-DMAPP) and p-hydroxyphenylpentazole(p-HPP) were synthesized at -40 ℃,using N1,N1-dimethylbenzene-1,4-diamine and 4-aminophenol as starting meaterials, respectively. Their stuctures were characterized by ¹H NMR, ¹³C NMR , ¹H-¹³C HMBC,¹⁵N NMR and ¹H-¹⁵N HMBC at low temperature. The results show that the ¹H NMR and ¹³C NMR data of p-DMAPP and p-HPP are in accordant with the literature values. Nitrogen signals of pentazole are assigned as N-1(δN -80.0), N-2/5(δN -27.3), N-3/4(δN 5.1) for p-DMAPP and N-1(δN -84.1), N-2/5(δN -28.1), N-3/4(δN 4.2) for p-HPP, respectively. 