Oxford as400 spectrometer

LC-MS data were obtained by Waters LCT Premier XE (High sensitive orthogonal acceleration time of flight device)-AQUITY ultra performance liquid chromatography system using Mass Lynx 4.1 software. 1D and 2D (COSY, HMBC, HSQC and NOESY) NMR spectra (400 MHz) were recorded on Varian Oxford AS400 spectrometer with TMS as internal standard at room temperature. Structures of the isolated compounds were given in Fig. 3.

MS data was acquired on a Thermo Scientific Accela1250 system consisting a mass detector (Thermo Scientific TSQ Quantum Access Maxx triple quadrupole). The mass analysis samples were dissolved in dichlorometane:methanol (1:1) at 10 ppm concentration, and 10 μL of this solution was directly injected to the instrument (Capillary Temperature: 400; Vaporizer Temperature: 500.0; Sheath Gas Pressure: 75.0; Ion Sweep Gas Pressure: 0.0; Aux Valve Flow: 20.0; Spray Voltage: Positive polarity -3000.0, Negative polarity -3000.0; Discharge Current: Positive polarity -4.0, Negative polarity -4.0). 1D and 2D NMR spectra were obtained at 400 MHz for 1 H and 100 MHz for 13 C on a Varian Oxford AS400 spectrometer, in CDCl 3 , with solvent peak used as reference. Column chromatography experiments were carried out on silica gel 60 (40-63 μm-Merck). TLC analyses were carried out on silica gel 60 F254 (Merck) and RP-18 F254s (Merck) plates. Compounds were detected by UV and 20% aq. H 2 SO 4 spraying reagent followed by heating at 105 °C for 1-2 min. For rotary evaporation, a Heidolph Laborota 4001 equipment was used.

IR spectra were obtained on a Perkin Elmer Spectrum 100 FT-IR spectrometer. Mass spectra analysis was carried out on Thermo-Scientific TSQ Quantum Access Max LC-MS/MS equipped with an ESI source. High Resolution Mass spectra were obtained on Agilent 6200 Series TOF and 6500 Series QTOF-MS system equipped with an ESI source. Optical rotation measurements were done on a Perkin Elmer Model-351 polarimeter in MeOH at 20 C. 1D and 2D (COSY, HMBC, HSQC and NOESY) NMR spectra were recorded on Varian Oxford AS400 spectrometer with TMS as internal standard at room temperature. 2D NMR spectra were run using standard Varian pulse programs. Column chromatography was carried out on silica gel 60 (40e63 mm-Merck), Sephadex LH-20 (GE Healthcare) and Lichroprep RP-C18 (25e40 mm, Merck) using analytical grade purity solvents (Merck and Sigma). TLC analyses were carried out on silica gel 60 F 254 and RP-C18 F 254s (Merck) pre-coated aluminum plates. Compounds were detected by UV (244e366 nm) and vanillin/H 2 SO 4 reagent followed by heating. Spraying with ninhydrin reagent followed by heating was used to detect the amino acid residue.