^(15)N标记的苯基五唑的合成、表征及分解反应机理

Synthesis,Characterization and Decomposition Reaction Mechanism of ^(15)N-Labelled Phenylpentazoles

以15 N标记的亚硝酸钠和叠氮化钠为原料,低温下合成出15 N标记的对甲氧基苯基五唑(p-MOPP)和对叔丁基苯基五唑(p-tBPP)。利用低温1 H NMR、13 C NMR和15 N NMR等一维核磁技术及gHSQC和gHMBC等二维核磁技术进行了p-tBPP的1 H、13 C、15 N NMR谱化学位移全归属。通过变温1 H NMR和15 N NMR研究了五唑化合物的稳定性,推测了其分解反应机理。

p-Methoxyphenylpentazole （p-MOPP） and p-tert-butylphenylpentazole （p-tBPP） were synthesized at low temperature, using is N-labelled NaNO2 and NaN3 as starting materials. The chemical shifts of 1 H,13 C and 12 N NMR spectra of p-tBPP were completely assigned by a combination of 1D （1H NMR,13C NMR and lS N NMR） and 2D （gHSQC and gHMBC） NMR techniques at low temperature. The stability of phenylpentazoles was studied by means of variable-temperature 18 NMR and 15 N NM1R. On the bases of the results of variable-temperature 15N NMR, the decomposition reaction mechanism of phenylpeatazoles was postulated.