Relevant articles and documents
Reaction monitoring by means of multivariate data analysis of near-infrared and raman spectra
Hetemi, Dardan Janagap, Steve
An efficient, versatile and non-destructive in situ method in reaction monitoring using vibrational spectroscopy is described. A Suzuki cross-coupling reaction was monitored in which the substrate 1-iodo-2-nitrobenzene reacted with the electrophile phenylboronic acid to form the product 2-nitrobiphenyl. To hasten the reaction, palladium(II) acetate and potassium carbonate were added to serve as catalyst and to promote transmetalation, respectively. This reaction was monitored using near-infrared and Raman spectroscopy. The recorded data was subjected to multivariate analysis such as principal component analysis in order to detect spectral changes due to the formation of the product. To confirm the presence of the desired product, offline analyses were performed using gas chromatography-mass spectrometry and nuclear magnetic resonance spectroscopy. The results demonstrate how Raman spectroscopy is able to detect the formation of the product in real time, whereas near-infrared spectroscopy fails to do so.
Regioselective mononitration of biphenyl by use of stoichiometric quantities of nitrogen dioxide and molecular oxygen over rare earth cationexchanged β-Zeolite catalysts
Tai, Yan Fang Dong, Xiong Zi Xu, Hao Shu Shi, Chun Jie Peng, Xin Hua
In the presence of molecular oxygen and zeolite La-b with Si/ Al2 = 260, regioselective mononitration of biphenyl with stoichiometric quantities of liquid nitrogen dioxide occurs at 20 °C to yield mononitrobiphenyl, as the main product, in yields up to 82.7 %. The 2-nitrobiphenyl:4-nitrobiphenyl isomer ratio is 0.34. The process is eco-friendly and inexpensive, and the zeolite is easily regenerated by simple work-up to give results similar to those obtained with the fresh catalyst.
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