Agilent q tof 6520 spectrometer

Commercially available reagents were used without further purification. Organic solvents were evaporated with reduced pressure using a Büchi R-100 evaporator (Büchi, Flawil, Switzerland). Reactions were monitored by TLC using Yantai JingYou (Yantai, China) GF254 silica gel plates. Silica gel column chromatography was performed on Biotage Isolera One (Biotage, Uppsala, Sweden). Melting points were measured by a Melting Point YRY-3 apparatus (Tianjin Precision Apparatus Factory, Tianjin, China). The purity of the samples was determined by an analytical Agilent 1260 HPLC (Agilent, Waldbronn, Germany) with ZDRBAX SB-C18 column (4.6 × 150 mm) using parameters as follows: H₂O/MeOH, 40/60 to 0/100 in 15 min, plus 5 min isocratic MeOH, flow rate at 1.0 mL/min, λ = 254 and 280 nm. NMR spectra were measured on Bruker Avance III 600 MHz spectrometer (Bruker, Fällanden, Switzerland). Chemical shifts were expressed in δ (ppm) and coupling constants (J) in Hz with residual solvent signals as references (CDCl₃, δ_H 7.26 ppm and δ_C 77.0 ppm; DMSO-d₆, δ_H 2.50 ppm and δ_C 39.5 ppm). ESIMS (electrospray ionization mass spectrometry) analyses were performed on an Agilent 1260-6460 Triple Quard LC-MS instrument (Agilent, Waldbronn, Germany). HR-ESIMS data were acquired on an Agilent Q-TOF 6520 spectrometer (Agilent, Waldbronn, Germany).

Melting points were measured by a Melting Point YRY-3 apparatus (Tianjin Precision Apparatus Factory, Tianjin, China). Commercially available reagents were used without further purification. Organic solvents were evaporated with reduced pressure using Büchi R-100 evaporators. Reactions were monitored by thin-layer chromatography (TLC) using Yantai JingYou (Yantai, China) GF254 silica gel plates. Silica gel column chromatography was performed on an Isolera One system (Biotage, Uppsala, Sweden) with and silica gel (200–300 mesh) from Qingdao Hailang Inc. (Qingdao, China). NMR spectra were measured on a BrukerAvance III 600 spectrometer (Bruker, Fällanden, Switzerland). Chemical shifts were expressed in δ (ppm) and coupling constants (J) in Hz, with residual solvent signals as internal standards (CDCl₃, δ_H 7.26 ppm and δ_C 77.0 ppm; DMSO-d₆, δ_H 2.50 ppm and δ_C 39.5 ppm). Electron spray ionization (ESI)-MS analyses were performed on an Agilent 1260-6460 Triple Quard LC-MS instrument and HR-ESI-MS data were acquired on an Agilent Q-TOF 6520 spectrometer (Agilent, Waldbronn, Germany).