6230 esi tof lc ms mass spectrometer

The reactions were performed using commercial reagents, and ACS grade solvents used for reactions were purified and dried in accordance with standard procedures. Column chromatography was performed on silica gel 60 (70–230 mesh), and reactions were monitored by TLC on Kieselgel 60 F254. The compounds were detected by examination under UV light and by charring with 5% sulfuric acid in methanol. Solvents were removed under reduced pressure at <40 °C. CH₂Cl₂ was distilled from CaH₂ directly prior to application. Pyridine was dried by refluxing with CaH₂ and then distilled and stored over molecular sieves (3 Å). Anhydrous DMF were used without further conditioning. Optical rotations were measured by using a Jasco P-1020 polarimeter. Unless noted otherwise, ¹H NMR spectra were recorded in CDCl₃ at 300 MHz (Bruker Advance) or at 500 MHz (Bruker ARX-500), ¹³C NMR spectra and two-dimensional experiments were recorded in CDCl₃ at 75 MHz (Bruker Advance) or at 125 MHz (Bruker ARX-500). The ¹H NMR chemical shifts are referenced to tetramethylsilane (TMS, δH = 0 ppm) or CDCl₃ (δH= 7.26 ppm) for ¹H NMR spectra for solutions in CDCl₃. The ¹³C NMR chemical shifts are referenced to the central signal of CDCl₃ (δC = 77.00 ppm) for solutions in CDCl₃. Accurate mass spectrometry determinations were performed using an Agilent 6230 ESI TOF LCMS mass spectrometer.

Column chromatography was performed on silica gel 60 (70–230 mesh), reactions were monitored by TLC on Kieselgel 60 F254. The compounds were detected by examination under UV light and by charring with 10% sulfuric acid in methanol. Solvents were removed under reduced pressure at <40 °C. CH₂Cl₂ and ClCH₂CH₂Cl (1,2-DCE) were distilled from CaH₂ directly prior to application. Pyridine was dried by refluxing with CaH₂ and then distilled and stored over molecular sieves (3 Å). Anhydrous DMF was used as it is. Molecular sieves (3 Å or 4 Å), used for reactions, were crushed and activated in vacuo at 390 °C during 8 h in the first instance and then for 2–3 h at 390 °C directly prior to application. Optical rotations were measured using a Jasco polarimeter. ¹H-NMR spectra were recorded in CDCl₃ at 300 or 600 MHz, ¹³C-NMR spectra were recorded in CDCl₃ at 75 or 151 MHz. Accurate mass spectrometry determinations were preformed using Agilent 6230 ESI TOF LCMS mass spectrometer

The reactions were performed using commercially available reagents. CH₂Cl₂ used for reactions was distilled from CaH₂ prior to the application. Other ACS-grade solvents used for reactions were purified and dried according to standard procedures. Prior to the initial application, silver salts were coevaporated with toluene (×2), dried in vacuo in the dark. Column chromatography was performed on silica gel 60 (70–230 mesh); reactions were monitored using Thin-Layer Chromatography (TLC) on Kieselgel 60 F₂₅₄. TLC was examined under UV light and by charring with 10% sulfuric acid in methanol. Solvents were removed under reduced pressure at <40 °C. Molecular sieves (3 Å) used for reactions were crushed and activated under vacuum for 8 h at 390 °C in the first instance, and then for 2–3 h at 390 °C directly prior to application. Optical rotations were measured by a Jasco P2000 polarimeter. ¹H and ¹³C NMR spectra were recorded in CDCl₃ at 300 and 75 MHz, respectively. ¹H NMR was calibrated to tetramethylsilane (TMS, δ_H = 0 ppm) in CDCl₃. ¹³C NMR was calibrated to the central signal of CDCl₃δ_c = 77.00 ppm) in CDCl₃. HRMS analysis was performed using an Agilent 6230 ESI TOF LC/MS mass spectrometer.