Vnmrs 300 mhz spectrometer

The 50 g of Amberlite® IRA-400 strongly basic ion exchange resin (chloride form, quaternary ammonium functional group) was packed in a plastic column and 100 mL of a 3% w/v methanolic solution of sodium ibuprofen (Na Ibu) was passed through the column in order to load the API molecule. The amount of Na Ibu remaining in the feed was found by UV-Vis spectroscopy which allowed the amount of Na Ibu loaded onto the resin to be calculated and the mass of counterion in the second step to be adjusted accordingly. Next, 100 mL of a 3% w/v solution containing 1-butyl-3-methyl imidazolium chloride (BMIm Cl) dissolved in methanol, acetonitrile, or dichloromethane was passed through the column. The eluent containing the API-IL was collected in fractions of 5 mL until no more API was detected in the solution. The reaction was carried out at room temperature using nitrogen to force the solutions through the packed bed at a flow rate of 30 mL min -1 . Fractions containing BMIm Ibu were combined and the solvent removed using a rotary evaporator. The product was then placed in a vacuum oven at 40 °C for 24 h to remove residual solvent. The 1:1 ratio between Ibu and BMIm ions was verified by 1 H NMR using a Varian VnmrS 300 MHz spectrometer.

Fourier-transform infrared (FTIR) spectra were collected in ATR mode on a Spectrum II Perkin-Elmer spectrometer. The powder X-ray diffraction (XRD) patterns were collected with a PANalytical X'Pert Pro MPD diffractometer (CuKα1 = 0.1540598 nm). The scanning electron microscopy (SEM) images were obtained with a Hitachi S-4800 electron microscope. The low-and high-resolution transmission electron microscopy (TEM) images were obtained using a JEOL JEM-ARM 200F transmission electron microscope. Nitrogen adsorption and desorption isotherms were measured at 77 K with a Micrometrics Triflex apparatus; the specific surface area was determined by the BET method, pore size distribution by the BJH method from the desorption branch or by DFT assuming cylindrical pore geometry. 1 H and 13 C NMR spectra in solution were recorded using a Bruker AVANCE 400 MHz spectrometer. Solid state 13 C CPMAS NMR spectra were recorded on a VARIAN VNMRS 300 MHz spectrometer using a 3.2 mm T3 2 channels probe. Rotors were spun at 12 kHz.