Ascend 500 11.75 tesla superconducting magnet

All the chemicals used were purchased form Sigma-Aldrich. IR spectroscopy studies were conducted on a Shimadzu IRAffinity-1 FTIR spectrometer calibrated against 1602 cm⁻¹ polystyrene absorbance spectra. The ¹H NMR and ¹³C NMR spectra were measured on a Bruker Avance III HD^® NMR spectrometer equipped with an Ascend 500 11.75 Tesla superconducting magnet, operating at 500.13 MHz for ¹H and 125.76 MHz for ¹³C, and a multinuclear 5 mm PABBO probe. Melting points were recorded on a Stuart^® SMP11 melting point apparatus. Reactions were monitored by TLC and GC. Mass spectra were measured via a Thermo Scientific GC/MS DSQ II device, which contained a column: EC-5 30 m × 0.25 mm i.d. × 0.25 µm or using the direct-infusion method using a Waters^® ACQUITY^® TQD system with a tandem quadrupole mass spectrometer. The software used was ThermoXcalibur 2.2 SP1.48. The XRF spectroscopy analysis of the catalyst was performed using a Bruker S2 Ranger^®.

All commercially available chemicals were purchased from Aldrich (St. Louis, MO, USA) and used without further purification. IR spectra were recorded on an IR Affinity-1 FTIR spectrometer (Shimadzu, Kyoto, Japan) calibrated against a 1602 cm⁻¹ polystyrene absorbance spectrum. Samples were analyzed as thin films in between sodium chloride discs. The ¹H NMR spectra were recorded on an Avance III HD^® NMR spectrometer (Bruker, Coventry, England), equipped with an Ascend 500 11.75 Tesla superconducting magnet, operating at 500.13 MHz for ¹H, and a multinuclear 5 mm PABBO probe (Bruker, Coventry, England). Samples were dissolved in the deuterated solvent specified in the section on the analytical information. Melting points of products were measured using a Stuart^® SMP11 melting point determination apparatus fitted with a mercury thermometer. Reactions were monitored using TLC plates composed of silica on PET with a fluorescent indicator and GC on a Shimadzu GC-2010 plus gas chromatograph equipped with a flame ionization detector and HiCap 5 GC column with dimensions of 0.32 mm (internal diameter) × 30 m (length) × 0.25 mm (film thickness), using nitrogen as carrier gas. Plates were observed under a UV lamp at a wavelength of 254 nm before staining in an iodine-saturated chamber.