Ftir ir prestige 21 spectrophotometer

The synthesized materials were characterized using FTIR, SEM, and XRD. SEM analyzes were performed using a Scanning Electron Microscope (SEM), model VEGA3 TESCAN (Kohoutovice, Czech Republic). The samples, which are all in the form of powder, were placed in stub-type sample holders with a fixation on double-sided tape with a black background. The materials were analyzed with magnifications between 1000× and 10,000×, at a voltage of 10 kV.
Fourier transform infrared spectroscopy analyses were carried out in a Shimadzu FTIR IR PRESTIGE 21 spectrophotometer (Kyoto, Japan), in the spectral range from 4000 to 400 cm⁻¹ with a resolution of 4 cm⁻¹ operating in transmittance mode with 50 scans using an analysis method with KBr (potassium bromide). Where tablets with 1 mg of sample to be analyzed and 100 mg of KBr were prepared, in addition to a tablet with only 100 mg of KBr, corresponding to the “blank sample”.
X-ray diffraction analyses were performed using a Shimadzu DRX 6000 model diffractometer (Kyoto, Japan). The samples were added in the form of powder and analyzed in the range from 5 to 90° with an interval of 0.02° (2θ) using copper radiation (Cu) with an X-ray source, where this corresponds to a wavelength of 0.15406 Å, using a voltage of 40 kV and a current of 30 mA.

The samples were ground with KBr powder and then pressed into tablets. FT-IR spectroscopy was recorded by using a Shimadzu Fourier transform (FT)/IR IRPRESTIGE-21 spectrophotometer in the frequency range of 4000–500 cm⁻¹ with the resolution of 4.0 cm⁻¹ and 320 scans co-addition [20 (link)].

The air- or moisture-sensitive reactions were performed under an argon atmosphere using dry glassware. All reagents, starting materials and solvents were purchased from commercial sources and used as received. TLC was performed on silica gel plates (60 F₂₅₄) and visualised under UV light (254 and 365 nm). Reversed-phase chromatography was done on a Biotage Isolera One system using Biotage SNAP KP-C18-HS cartridges. Melting points were determined on an OptiMelt MPA100 apparatus. IR spectra were recorded on a Shimadzu FTIR IR Prestige-21 spectrophotometer. ¹H, ¹³C and ³¹P NMR spectra were recorded on a Bruker Avance Neo 400 MHz spectrometer. The chemical shifts (δ) were reported in parts per million (ppm) relative to the residual solvent peak as an internal reference (DMSO-d₆: ¹H 2.50, ¹³C 39.52; CD₃OD: ¹H 3.31, ¹³C 49.00). ³¹P shifts were referenced externally to H₃PO₄. The coupling constants (J) were expressed in Hertz (Hz). HRMS was performed on a Q-TOF Micro mass spectrometer.
The synthesis and characterisation of 4-iodo-2-vinylphenol (2a), 2-bromo-6-vinylphenol (2c), ethyl allylphosphonochloridate (3), ethyl (4-iodo-2-vinylphenyl) allylphosphonate (4a), 2-bromo-6-vinylphenyl ethyl allylphosphonate (4c) together with corresponding 3H-1,2-benzoxaphosphepine 2-oxides 6a,c and 7a,c are reported by our group in the previous paper¹⁹ (link).