Lcq xp

¹H and ¹³C NMR spectra (CDCl₃, CD₃OD or DMSO-d₆) were recorded on Bruker AV 400 (400/100 MHz), Bruker AMX 500 (500/125 MHz), or Jeol JNM-ECA600 (600/150 MHz) instrument. Chemical shifts are reported as parts per million (δ) relative to the solvent peak. Coupling constants (J) are reported in hertz (Hz). Mass spectra were recored on a Thermo LCQ XP instrument. Optical rotations were determined on Jasco III in appropriate solvent. UV spectra were recorded on U-3000 made by Hitachi in methanol or water. Infrared spectra were recorded on FT-IR (FTS-135) made by Bio-Rad. Melting points were determined on a Buchan B-540 instrument and are uncorrected. Elemental analyses (C, H, and N) were used to determine the purity of all synthesized compounds, and the results were within ± 0.4% of the calculated values, confirming ≥ 95% purity. Reactions were checked with TLC (Merck precoated 60F254 plates). Flash column chromatography was performed on silica gel 60 (230-400 mesh, Merck). Unless otherwise noted, materials were obtained from commercial suppliers and were used without purification. All solvents were purified and dried by standard techniques just before use. THF and Et₂O were freshly distilled from sodium and benzophenone. Methylene chloride, toluene, and benzene were purified by refluxing with CaH₂. Hexanes and ethylacetate were purified by simple distillation.

Proton (¹H) and carbon (¹³C) NMR spectra were obtained on a Bruker AV 400 (400/100 MHz), Bruker AMX 500 (500/125 MHz), Jeol JNM-ECA600 (600/150 MHz), or Bruker AVANCE III 800 (800/200 MHz) spectrometer. Chemical shifts are reported as parts per million (δ) relative to the solvent peak. Coupling constants (J) are reported in hertz (Hz). Mass spectra were recorded on a Thermo LCQ XP instrument. Optical rotations were determined on Jasco III in appropriate solvent. UV spectra were recorded on U-3000 made by Hitachi in methanol or water. Infrared spectra were recorded on Fourier transform infrared (FT-IR; FTS-135) made by Bio-Rad. Melting points were determined on a Buchan B-540 instrument and are uncorrected. The crude compounds were purified by column chromatography on a silica gel (Kieselgel 60, 70–230 mesh, Merck). Elemental analyses (C, H, and N) were used to determine the purity of all synthesized compounds, and the results were within ±0.4% of the calculated values, confirming ≥95% purity. High-performance liquid chromatography (HPLC) analysis was also performed to determine the purity of the final compounds 6a–c, confirming ≥95% purity.