CAJ | 학술논문

利用在线红外技术监测3,4-双(4'-氨基呋咱基-3')氧化呋咱(DATF)的合成过程,并结合核独立成分分析算法对反应过程中获得的实时红外光谱数据进行解析,得到了反应物、中间体及产物各组分纯物质的红外光谱图。采用密度泛函理论B3LYP法,在6-31+G( d,p)基组水平上求得中间体的红外振动光谱,验证了所分离红外光谱图的正确性,从而推导出合理的合成反应机理。结果表明,核独立成分分析算法能合理地解析红外光谱在线数据,并有效捕捉合成反应的中间体,对合成反应机理的研究具有重要的指导意义。
이용재선홍외기술감측3,4-쌍(4'-안기부찰기-3')양화부찰(DATF)적합성과정,병결합핵독립성분분석산법대반응과정중획득적실시홍외광보수거진행해석,득도료반응물、중간체급산물각조분순물질적홍외광보도。채용밀도범함이론B3LYP법,재6-31+G( d,p)기조수평상구득중간체적홍외진동광보,험증료소분리홍외광보도적정학성,종이추도출합리적합성반응궤리。결과표명,핵독립성분분석산법능합리지해석홍외광보재선수거,병유효포착합성반응적중간체,대합성반응궤리적연구구유중요적지도의의。
On-line infrared(IR) spectroscopy was used to monitor the synthesis process of 3,4-bis(4’-ami-nofurazano-3’) furoxan(DATF). The IR spectra of components were determined by analyzing the IR data using principal component analysis( PCA) and independent component analysis( ICA) . The geometric configu-rations of intermediates were optimized using the density functional theory(DFT) at B3LYP/6-31+G(d,p) level. Their vibrational frequencies of IR spectra were obtained on the basis of vibrational analysis. The result obtained by the chemometric resolution methods agreed well with that of quantum chemical calculation method, which demonstrated the reliability of the proposed chemometric resolution methods. The unstable intermediate was confirmed via comparing the IR spectra that calculated using B3LYP/6-31+G(d,p) and analyzed by ICA. Finally, the possible synthesis mechanism of DATF was deduced based on the analysis of the above IR spec-tra. The above mentioned work was expected to provide significant guidance to investigate the reaction mecha-nism in the future.