Isolera spektra systems

¹H and ¹³C NMR data were recorded on a Bruker (Billerica, MA, USA) 400 spectrometer. ¹H NMR data are reported as follows: chemical shift in ppm (δ), multiplicity (s = singlet, d = doublet, t = triplet, m = multiplet), coupling constant (Hz), relative intensity. ¹³C NMR data are reported as follows: chemical shift in ppm (δ). HPLC-MS analyses were performed on a Shimadzu-2020 LC-MS instrument (Kyoto City, Japan) using the following conditions: Shim-pack VPODS C18 column (reverse phase, 150 × 2.0 mm); 80% acetonitrile and 20% water over 6.0 min; flow rate of 0.4 mL/min; UV photodiode array detection from 200 to 300 nm. The products were purified using Biotage (Uppsala, Sweden) Isolera™ Spektra Systems and hexane/EtOAc solvent systems. Unless otherwise specified, all chemicals were purchased from commercial sources and used without further treatment. All microwave irradiation experiments were carried out according to our previous report [44 (link),45 (link)].

¹H and ¹³C NMR were recorded on a Bruker 400 spectrometer. ¹H NMR data are reported as follows: chemical shift in ppm (δ), multiplicity (s = singlet, d = doublet, t = triplet, m = multiplet), coupling constant (Hz), relative intensity. ¹³C NMR data are reported as follows: chemical shift in ppm (δ). HPLC-MS analyses were performed on a Shimadzu-2020 LC-MS instrument using the following conditions: Shim-pack VPODS C18 column (reverse phase, 150 × 2.0 mm); 80% acetonitrile and 20% water over 6.0 min; flow rate of 0.4 mL/min; UV photodiode array detection from 200 to 300 nm. The reaction was irradiated at the required ceiling temperature (the reaction temperature was monitored by an external surface sensor using the Biotage Initiator reactor) using maximum power for the stipulated time. Then it was cooled to 50 °C with gas jet cooling. The products were purified by Biotage Isolera™ Spektra Systems and Hexane/EtOAc solvent systems. All reagents and solvents were obtained from commercial sources and used without further purification.