6210a lc tof instrument

Commercially available reagents and solvents were used without further purification. All reactions were monitored by thin-layer chromatography (TLC) using 0.25 mm Silicycle extra hard 250 µM TLC plates (60 F254). Purification of reaction products was carried out by flash chromatography using an Agilent 971-FP flash purification system with Silicycle silica gel columns. The yields are not optimized. The purity of all compounds was over 95% as analyzed with an Agilent 1260 Infinity HPLC system and an Agilent Poroshell 120 EC-C18 (4.6 × 50 mm, 2.7 µm) reverse phase column, detecting with UV absorbance (254 nm). ¹H NMR and ¹³C NMR spectra were obtained using a Bruker Avance III 500 MHz system (500 MHz for ¹H NMR and 125 MHz for ¹³C NMR) spectrometer. Chemical shifts are reported relative to chloroform (δ = 7.26 for ¹H NMR and δ = 77.16 for ¹³C NMR spectra) or dimethyl sulfoxide (δ = 2.50 for ¹H and δ = 39.52 for ¹³C NMR spectra). Data are reported as br = broad, s = singlet, d = doublet, t = triplet, q = quartet, m = multiplet. Mass spectra were obtained using a Bruker AmaZon SL system. High resolution mass spectra (HRMS) were performed using an Agilent 6210A LC-TOF instrument with a dual spray ESI source, with a high resolution Time of Flight (TOF) Mass analyzer and collecting in a 2GigHz detector mode, coupled with an Agilent 1200 HPLC.

Commercially available reagents and solvents were used without further purification. All reactions were monitored by thin-layer chromatography (TLC) using 0.25 mm Silicycle extra hard 250 μM TLC plates (60 F254). Purification of reaction products was carried out by flash chromatography using an Agilent 971-FP flash purification system with Silicycle silica gel columns. The yields are not optimized. The purity of all compounds was >95% as analyzed with an Agilent 1260 Infinity HPLC system. 1H NMR and ¹³C NMR spectra were obtained using a Bruker Avance III 500 MHz system (500 MHz for ¹H NMR and 125 MHz for ¹³C NMR) or Agilent DD MR-400 system (400 MHz for ¹H NMR and 100 MHz for ¹³C NMR) spectrometer. Chemical shifts are reported relative to chloroform (δ = 7.26 for 1H NMR and δ = 77.16 for 13C NMR spectra) or dimethyl sulfoxide (δ = 2.50 for ¹H and δ = 39.52 for ¹³C NMR spectra). Data are reported as br = broad, s = singlet, d = doublet, t = triplet, q = quartet, m = multiplet. Mass spectra were obtained using a Bruker AmaZon SL system. High resolution mass spectra (HRMS) were performed using an Agilent 6210A LC-TOF instrument with a dual spray ESI source with a high resolution time of flight (TOF) mass analyzer and collecting in a 2GigHz detector mode coupled with an Agilent 1200 HPLC.