The general protocols employed in the synthetic procedures, structure elucidation of the new chemical structures, and purity of the newly synthesized lapatinib derivatives were performed as reported earlier, with some modifications [37 (
link),38 (
link),39 (
link),40 (
link)]. In brief, all acquired solvents and reagents were utilized without additional purification. Dimethyl sulfoxide (DMSO) was used as a solvent for NMR analysis.
1H NMR spectra were acquired using Bruker
400 MHz spectrometer, with chemical shifts being determined in parts per million (ppm) and coupling constants in Hz.
13C NMR spectra were acquired using Varian 100 MHz spectrometer (Varian Medical Systems, Inc., Palo Alto, CA, USA). The
G2 QTOF mass spectrometer (Waters Corporation, Milford, MA, USA) was employed to produce the mass spectra, high-resolution mass spectrometry (HRMS, ESI-MS). Reaction monitoring was performed using TLC on 0.25 mm silica plates (E. Merck; silica gel 60 F
254). To verify the purity of the target compounds, high-performance liquid chromatography (HPLC); System: Waters Corp. 2695 with PAD 996, λ = 281 nm; Column: Welch Xtimate C
18 150 mm × 4.6 mm × 5 μm; Condition: mobile phase A: 0.05% TFA in water, mobile phase B: CH
3CN; Gradient: 90% of Mobile phase B in 30 min. The melting points (M.p.) were assessed with Thermo Scientific 9200 (Rise 10 °C per minute).
Elkamhawy A., Son S., Lee H.Y., El-Maghrabey M.H., Hamd M.A., Alshammari S.O., Abdelhameed A.A., Alshammari Q.A., Abdeen A., Ibrahim S.F., Mahdi W.A., Alshehri S., Alnajjar R., Choi W.J., Al-Karmalawy A.A, & Lee K. (2022). Design, Synthesis, Biological Evaluation, and Molecular Dynamics Studies of Novel Lapatinib Derivatives. Pharmaceuticals, 16(1), 43.