6230 tof lc ms spectrometer

All commercial chemicals were used as supplied unless otherwise indicated. Flash chromatography was performed on a Teledyne Combiflash RF-200 with RediSep columns (silica) and indicated mobile phase. All moisture sensitive reactions were performed under an inert atmosphere of ultrapure argon with oven-dried glassware. ¹H and ¹³C NMR spectra were recorded on a Varian 600 MHz or Bruker 400 spectrometer. Mass data were acquired on an Agilent 6230 TOF LC/MS spectrometer capable of ESI and APCI ion sources. Analysis of sample purity was performed on a Varian Prepstar SD-1 HPLC system with a Phenomenex Gemini, 5 μm C18 column (250 mm × 4.6 mm). HPLC conditions: solvent A = H₂O, solvent B = MeCN; flow rate = 1.0 mL/min; compounds were eluted with a gradient of 20% MeCN/H₂O to 100% MeCN for 30 min. Purity was determined by total absorbance at 254 nm. All tested compounds have a purity ≥ 97%.
Deazaflavin analogues (4a-d) were reported earlier by Raoof et al.^{15 (link)}

All commercial chemicals were used as supplied unless otherwise indicated. Microwave synthesis was performed with a Biotage Initiator Microwave Synthesizer. Flash chromatography was performed on a Teledyne Combiflash RF-200 with RediSep columns (silica) and indicated mobile phase. All moisture sensitive reactions were performed under an inert atmosphere of ultra-pure argon with oven-dried glassware. ¹H and ¹³C NMR spectra were recorded on a Varian 600 MHz or Bruker 400 spectrometer. Mass data were acquired using an Agilent 6230 TOF LC/MS spectrometer. All NMR and mass spectrometers are located in the shared instrument rooms at the Center for Drug Design, University of Minnesota. Analysis of sample purity was performed on a Agilent Varian Prepstar SD-1 HPLC system located in our own lab with a Phenomenex Gemini, 5 ¼m C18 column (250mm × 4.6 mm). HPLC conditions: solvent A: H₂O with 0.1% TFA; solvent B: MeCN; flow rate 1.0 mL/min; compounds were eluted with a gradient of 20% MeCN/H₂O with 0.1% TFA to 100% MeCN for 20 min. All tested compounds have a purity ≥ 97%.

All commercial chemicals were used as supplied unless otherwise indicated. Flash chromatography was performed on a Teledyne Combiflash RF-200 with RediSep columns (silica) and indicated mobile phase. All moisture sensitive reactions were performed under an inert atmosphere of ultra-pure argon with oven-dried glassware. ¹H and ¹³C NMR spectra were recorded on a Varian 600 or Bruker 400 MHz spectrometers. Mass data were acquired using an Agilent 6230 TOF LC/MS spectrometer. Melting points were taken using Electrothermal Mel-Temp melting point apparatus. Compound purity analysis was performed using Agilent 1260 Infinity HPLC with an Eclipse C18 column (3.5 μm 4.6×100 mm). HPLC conditions: Flow rate = 1.0 mL/min; Solvent A = 0.1% TFA in water; Solvent B = 0.1% TFA in acetonitrile; Gradient (B %): 0–6 min (5–100); 6–8 min (100); 8–9 min (100–5). Determined purity was > 95% for all final compounds.

General procedures. All commercial chemicals were used as supplied unless otherwise indicated. Flash chromatography was performed on a Teledyne Combiflash RF-200 with RediSep columns (silica) and indicated mobile phase. All moisture-sensitive reactions were performed under an inert atmosphere of ultra-pure argon with oven-dried glassware. ¹H and ¹³C NMR spectra were recorded on Varian 600 or Bruker 400 MHz spectrometers. Mass data were acquired using an Agilent 6230 TOF LC/MS spectrometer.

All commercial chemicals were used as supplied unless otherwise indicated. Flash chromatography was performed on a Teledyne Combiflash RF-200 with RediSep columns (silica). All moisture sensitive reactions were performed under an inert atmosphere of ultra-pure argon with oven-dried glassware. 1H and 13C NMR spectra were recorded on a Varian 600 MHz spectrometer. Mass data were acquired using an Agilent 6230 TOF LC/MS spectrometer. Analysis of sample purity was performed on a Varian Prepstar SD-1 HPLC system with a Phenomenex Gemini, 5 µm C18 column (250mm × 4.6 mm). HPLC conditions: solvent A: H₂O with 0.1% TFA; solvent B: MeCN; flow rate 1.0 mL/min; compounds were eluted with a gradient of 20% MeCN/H₂O with 0.1% TFA to 100% MeCN for 20 min. All tested compounds have a purity ≥ 95%.

All chemical reagents and solvents were purchased from Sigma-Aldrich and used without further purification. Water (18 MΩ) was purified using a Millipore Analyzer Feed System. Solid-phase resins were purchased from Advanced ChemTech and Chem-Impex International.
Reversed-phase high-performance liquid chromatography (RP-HPLC) was performed using a Shimadzu system equipped with a CBM-20A communications bus module, two LC-20AT pumps, an SIL-20A auto sampler, an SPD-20A UV/vis detector, a CTO-20A column oven, and an FRC-10A fraction collector. Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) data were obtained on a Bruker Microflex spectrometer equipped with a 60 Hz nitrogen laser and a reflectron. In positive ion mode, the acceleration voltage on Ion Source 1 was 19.01 kV. Exact mass (EM) data were obtained on an Agilent Technologies 6230 TOF LC/MS spectrometer. The samples were sprayed with a capillary voltage of 3500 V, and the electrospray ionization (ESI) source parameters were as follows: gas temperature of 325 °C at a drying gas flow rate of 8 L/ min at a pressure of 35 psi.