Synthesis,GC-EIMS,~1H NMR,~(13)C NMR,Mechanistic and Thermal Studies of o-Xylylene-α,α'-bis (tr

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Organophosphorous compounds containing phosphorus as an integral part have been widely used in industry, organic synthesis and optoelectronics. o-Xylylene-α,α’-bis(triphenylphosphinebromide)(OXBTPPB) is a facile reagent to convert o-quinones(e.g., 9,10-phenanthrenequinone) into polycyclic aromatic hydrocarbons(PAHs). Herein lies an improved synthetic route to OXBTPPB. The resultant was carefully characterized with GC-EIMS, 1H NMR, 13C NMR, spectroscopic techniques. The EIMS shows characteristic peaks at m/z=262.4, 183.3, 108.2, 77.1 attributed to the [C18H15P]+·, [C12H8P]+, [C6H5P]+, [C6H5]+ ions, respectively. The 1H and 13C NMR spectrum shows well resolved peaks and all the hydrogens and carbons were well-assigned via a combined study of 1H-1H COSY, HMBC, and HMQC experiments. The mechanism for the formation of OXBTPPB was proposed based on literature and obtained experimental data. Meanwhile, the thermal stability of OXBTPPB was evaluated with TGA analysis, and an onset decomposition temperature(Td) was recorded at 323.6 °C. Organophosphorous compounds containing phosphorus as an integral part have been widely used in industry, organic synthesis and optoelectronics. O-Xylylene-α, α’-bis (triphenylphosphinebromide) (OXBTPPB) is a facile reagent to convert o-quinones 10-phenanthrenequinone into polycyclic aromatic hydrocarbons (PAHs). Herein lies an improved synthetic route to OXBTPPB. The resultant was carefully characterized by GC-EIMS, 1H NMR, 13C NMR, spectroscopic techniques. The EIMS shows characteristic peaks at m / z = The1H and13C NMR spectra show well resolved peaks and all the hydrogens and carbons (C12H8P) +, [C6H5P] +, [C6H5] + ions, respectively. were well-assigned via a combined study of 1H-1H COZY, HMBC, and HMQC experiments. The mechanism for the formation of OXBTPPB was proposed based on literature and obtained experimental data. Meanwhile, the thermal stability of OXBTPPB was evaluated with TGA analysis, and an onset decomposi tion temperature (Td) was recorded at 323.6 ° C.
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