G2 qtof mass spectrometer

In the conducted experiments all acquired solvents and reagents were applied without additional purification. Varian 400 MHz spectrometer (Varian Medical Systems, Inc., Palo Alto, CA, USA) was utilised to calculate the ¹H NMR spectra with chemical shifts being measured in parts per million (ppm) and coupling constants in Hz. The high-resolution electrospray ionisation mass spectrometry (HR-ESIMS) data were assessed utilising a JMS–700 mass spectrometer (Jeol, Japan) or by HR-ESIMS data obtained via a G2 QTOF mass spectrometer. Reaction monitoring was carried out using TLC on 0.25 mm silica plates (E. Merck; silica gel 60 F₂₅₄). Reverse-phase high performance liquid chromatography (RP-HPLC) was employed to determine the purity of the products, with the UV detector of the HPLC being set at 254 nm. The mobile phases employed were: (A) H₂O containing 0.05% TFA and (B) CH₃CN. The purity of the final compound was determined using a gradient of 75% B or 100% B in 30 min. The melting points were measured using a Fisherbrand digital melting point apparatus. Compounds 2a–b and 3a–d were synthesised as reported earlier³⁴ (link). The final target compounds were synthesised following the reported procedure of Suzuki cross-coupling reaction³⁴ (link).

All the chemicals, reagents, and solvents were purchased from commercial suppliers and used without purification, unless otherwise noted. Reactions were monitored by analytical TLC carried out using glass sheets pre-coated with Silica Gel 60 F₂₅₄ purchased from Merck, with visualization under UV light (254 nm). The NMR spectra were obtained on Bruker Avance 400. Column chromatography was performed on Merck Silica Gel 60 (230–400 mesh). The high-resolution electrospray ionization mass spectrometry (HR-ESIMS) data were recorded on a JMS-700 mass spectrometer (Jeol, Japan) or by HR-ESIMS data recorded on a G2 QTOF mass spectrometer. Product purity was determined by reversed-phase high-performance liquid chromatography (RP-HPLC) using a Waters Corp. HPLC system equipped with a UV detector set at 254 nm. The mobile phases used were: (A) H₂O containing 0.05% TFA and (B) CH₃CN. HPLC employed a YMC Hydrosphere C18 (HS-302) column (5 μm particle size, 12 nm pore size) that was 4.6 mm in diameter × 150 mm in size with a flow rate of 1.0 mL/min. The compound purity was assessed using either a gradient of 25% B or 100% B in 30 min (method A).