Sio2 60 f254 tlc

All reagents and solvents were used as supplied without further purification unless otherwise noted. Anhydrous solvents are dried over 4 Å molecular sieves. 0.7 M ZnCl₂ solution in THF was purchased from Arcos Organics and used without change. Preparative TLC (PTLC) and column chromatography were conducted using Millipore SiO₂ 60 F254 PTLC (0.5 mm) and Zeochem ZEOprep 60 ECO SiO₂ (40–63 μm), respectively. Analytical TLC was conducting using Millipore SiO₂ 60 F254 TLC (0.250 mm) plates. ¹H, ¹³C and ¹⁹F NMR spectra were obtained on a Bruker Avance III HD 600 MHz spectrometer equipped with either a 5 mm QCI or 5 mm CPDCH probe, a Bruker Avance III 500 MHz spectrometer equipped with a 5 mm BBFO probe, or a Bruker Avance III 400 MHz spectrometer equipped with a 5 mm BBFO probe. Chemical shifts are referenced to residual solvent (CDCl₃, δ 7.26 (¹H) and 77.0 (¹³C); CD₂Cl₂, δ 5.32 (¹H) and 54.2 (¹³C); (CD₃)₂CO, δ 2.09 (¹H) and 205.9 (¹³C)). IR spectra were obtained on a Thermo Nicolet 380 FT-IR with a SmartOrbit Diamond ATR accessory. Mass spectrometry analysis was performed by direct sample injection on an Agilent G1969A ESI-TOF mass spectrometer. The single crystal X-ray diffraction studies were carried out on a Bruker Kappa APEX-II CCD diffractometer equipped with Mo K_α radiation (λ = 0.71073 Å). Melting points (mp) are uncorrected.

All reagents and solvents were used as supplied without further purification unless otherwise noted. All reactions were performed in anhydrous solvents unless otherwise noted. CHCl₃ was pre-treated with alumina for at least 24 h prior to use. Preparative TLC (PTLC) and column chromatography were conducted using Millipore SiO₂ 60 F₂₅₄ PTLC (0.5 mm) and Zeochem ZEOprep 60 ECO SiO₂ (40–63 μm), respectively. Analytical TLC was conducting using Millipore SiO₂ 60 F254 TLC (0.250 mm) plates. ¹H and ¹³C NMR spectra were obtained using a Bruker Avance III HD 600 MHz spectrometer equipped with either a 5 mm QCI or 5 mm CPDCH probe or a Bruker Avance III 500 MHz spectrometer equipped with a 5 mm BBFO probe. IR spectra were obtained using a Thermo Nicolet 380 FT-IR with a SmartOrbit Diamond ATR accessory. Mass spectrometry analysis was performed by direct sample injection on an Agilent G1969A ESI-TOF mass spectrometer.

All reagents and solvents were used as supplied without further purification unless otherwise noted. CHCl₃ was pre-treated with alumina for at least 24 h prior to use. Amidines were purchased as their hydrochloride salts and free-based by treatment with 2 M KOH (aq). Enamines and ynamines were prepared as reported in the literature.^{53 –58} Preparative TLC (PTLC) and column chromatography were conducted using Millipore SiO₂ 60 F₂₅₄ PTLC (0.5 mm) and Zeochem ZEOprep 60 ECO SiO₂ (40–63 μm), respectively. Analytical TLC was conducted using Millipore SiO₂ 60 F254 TLC (0.250 mm) plates. ¹H and ¹³C NMR spectra were obtained on a Bruker Avance III HD 600 MHz spectrometer equipped with either a 5 mm QCI or 5 mm CPDCH probe. IR spectra were obtained on a Thermo Nicolet 380 FT-IR with a SmartOrbit Diamond ATR accessory. Mass spectrometry analysis was performed by direct sample injection on an Agilent G1969A ESI-TOF mass spectrometer. Melting points are uncorrected. The single-crystal X–ray diffraction studies were carried out on a Bruker Kappa APEX-II CCD diffractometer equipped with Mo Kα radiation (λ = 0.71073).