In situ ATR-FTIR combined with SIMPLISMA algorithm to investigate the synthesis mechanism of 4-amino-3,5-dimethyl pyrazole
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- 作者：Xinyu Gao ; Junxiu Ma ; Fangqi Ruan…
- 关键词：4 ; Amino ; 3 ; 5 ; dimethyl pyrazole ; Synthesis mechanism ; In situ attenuated total refletion ; Fourier transform infrared spectroscopy(ATR ; FTIR) ; Simple ; to ; use interactive self ; modelling mixture analysis(SIMPLISMA) algorithm ; Density functional theory
- 刊名：Chemical Research in Chinese Universities
- 出版年：2016
- 出版时间：December 2016
- 年：2016
- 卷：32
- 期：6
- 页码：985-991
- 全文大小：
- 刊物主题：Chemistry/Food Science, general; Analytical Chemistry; Inorganic Chemistry; Organic Chemistry; Physical Chemistry;
- 出版者：Jilin University and The Editorial Department of Chemical Research in Chinese Universities
- ISSN：2210-3171
- 卷排序：32
文摘
In situ attenuated total refletion-Fourier transform infrared spectroscopy(ATR-FTIR) was used to monitor and acquire spectral information on the synthesis of 4-amino-3,5-dimethyl pyrazole. Principal component analysis(PCA) was used to determine the number of principle components(PCs). The score vectors of the PCs were analysed using the simple-to-use interactive self-modelling mixture analysis(SIMPLISMA) algorithm to obtain spectral and concentration profiles for the reactants, intermediates and product. The vibrational frequencies of the intermediates were calculated via density functional theory(DFT) at the level of the B3LYP/6-311++G(d,p) basis set, and the geometrical configurations of the intermediates were simultaneously optimized. Finally, a reasonable synthesis mechanism for 4-amino-3,5-dimethyl pyrazole was determined based on the changes observed in the feature peaks. The results from the SIMPLISMA algorithm correlated well with the quantum chemistry calculations. This proved that the SIMPLISMA algorithm combined with ATR-FTIR can be used to determine the synthesis mechanism for 4-amino-3,5-dimethyl pyrazole and can even provide a new, useful method to explore dynamic synthesis reaction mechanisms.