Reagents and solvents were purchased from commercial sources and were used without further purification. All reaction were monitored by thin-layer chromatography (TLC) and visualized with UV light. Melting points were determined on an X-5 micromelting apparatus (Haohai Inc., Nanjing, China) and are uncorrected. 1H NMR and 13C NMR spectra were recorded on a Bruker 400 and 100 MHz spectrometer (Ettlingen, Germany), respectively. High resolution mass spectra (HR-MS) were recorded on a Waters Micromass Q-T of Micromass spectrometer (Milford, MA, USA) by electrospray ionization (ESI). Final products were of >95% purity as analyzed by HPLC analysis (Phenomenex column, C18, 5.0 μm, 150 mm × 4.6 mm) on Dionex UltiMate 3000 UHPLC instrument from ThermoFisher (Waltham, MA, USA). The signal was monitored at 254 nm with a UV dector. A flow rate of 1.0 mL/min was used with a mobile phase of methanol in H2O (80:20, v/v).
Dionex ultimate 3000 uhplc instrument
Manufactured by Thermo Fisher Scientific
Sourced in United States
The Dionex Ultimate 3000 UHPLC+ instrument is a high-performance liquid chromatography system designed for advanced analytical applications. It features a modular design and offers enhanced performance capabilities for complex separations and sensitive detection.
Automatically generated - may contain errors
3 protocols using dionex ultimate 3000 uhplc instrument
1
Characterization of Organic Compounds
2
UHPLC-PDA and NMR Analysis of Compounds
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HPLC analysis were carried out using a Thermo Scientific Dionex Ultimate 3000 UHPLC+ instrument (Thermo Scientific, Waltham, MA, USA) with a photodiode array detector (detection in wavelength: 210–450 nm). A C-18 analytical column ZORBAX Eclipse XDB (5 µm, 4.6 × 250 mm, Agilent, Santa Clara, CA, USA) was used at the flow rate of 1 mL/min. Chromatographic separation was achieved using the isocratic elution of 50% A (0.05% formic acid water solution) and 50% B (methanol containing 0.05% of formic acid) for 2 min, then linear gradient of B from 50% to 95% for 10 min and isocratic elution of 95% B for 2 min.
The obtained products were identified using nuclear magnetic resonance (NMR) spectroscopy. 1H-NMR, 13C-NMR, 1H-1H-NMR (COSY), and 1H-13C-NMR (HSQC, HMBC) spectra analyses were recorded using a DRX Bruker Avance TM 600 (600 MHz) instrument.
The obtained products were identified using nuclear magnetic resonance (NMR) spectroscopy. 1H-NMR, 13C-NMR, 1H-1H-NMR (COSY), and 1H-13C-NMR (HSQC, HMBC) spectra analyses were recorded using a DRX Bruker Avance TM 600 (600 MHz) instrument.
3
UHPLC Analysis of Compounds
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A Thermo Scientific Dionex Ultimate 3000 UHPLC+ instrument (Thermo Scientific, Waltham, MA, USA) with a photodiode array detector (detection in wavelength: 210–450 nm) with a C-18 analytical column ZORBAX Eclipse XDB (5 µm, 4.6 × 250 mm, Agilent, Santa Clara, CA, USA) was used to performed UHPLC analyses. Chromatographic separation was achieved using an isocratic elution of 50% A (0.05% formic acid water solution) and 50% B (methanol containing 0.05% of formic acid) for 2 min, then a linear gradient of B from 50% to 95% for 10 min and isocratic elution of 95% B for 5 min. The flow rate was 1.0 mL/min.
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