All reagents were of commercial quality. Solvents were dried and purified by standard methods. Analytical TLC was performed on aluminum sheets coated with a 0.2 mm layer of silica gel 60 F254. Silica gel 60 (230–400 mesh) was used for flash chromatography. Analytical HPLC-MS was performed on Waters equipment coupled to a single quadrupole ESI-MS (Waters Micromass ZQ 2000) using a reverse-phase SunFire C18 4.6 × 50 mm column (3.5 μm) at a flow rate of 1 mL/min and by using a diode array UV detector. Mixtures of CH3CN and H2O were used as mobile phases (gradient of 15−95% of acetonitrile in water, as indicated in each case). HRMS (EI+) was carried out on Agilent 6520 Accurate-Mass Q-TOF LC/MS equipment. NMR spectra were recorded on a Bruker-AVANCE 300, a Varian-INOVA 400, and VARIAN SYSTEM-500 spectrometer. Melting points were determined on a Mettler MP70 apparatus and are uncorrected.
Micromass zq 2000
Manufactured by Waters Corporation
The Micromass ZQ 2000 is a compact, high-performance mass spectrometer designed for routine analysis. It features an electrospray ionization (ESI) source and a quadrupole mass analyzer to provide accurate mass measurement. The system is suitable for a variety of applications, including pharmaceutical, environmental, and food analysis.
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2 protocols using micromass zq 2000
1
Analytical Characterization of Organic Compounds
2
Purification and Characterization of Organic Compounds
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CH3CN was dried by reflux over CaH2. Anhydrous DMF and reagents were obtained from commercial sources and used without further purification. Analytical thin-layer chromatography (TLC) was performed on silica gel 60 (F254; Merck). Compounds were purified by flash column chromatography with silica gel 60 (230 to 400 mesh) (Merck). The purity of the compounds was analyzed using a high-performance liquid chromatography mass spectrometer (HPLC-MS) and was performed on an HPLC Waters 2695 instrument connected to a Waters Micromass ZQ 2000 spectrometer and a photodiode array detector. The column used was a Sunfire C18 (4.6 mm by 50 mm, 3.5 mm), and the flow rate was 1 mL min−1. All retention times are quoted in minutes. Nuclear magnetic resonance (NMR) spectra were recorded with Varian XL-400 spectrometer operating at 400 MHz for 1H-NMR and at 100 MHz for 13C with Me4Si as an internal standard. Mass spectra were measured on a quadrupole mass spectrometer equipped with an electrospray source (LC/MC HP1100; Hewlett-Packard). Microanalyses were obtained on a Heraeus CHN-O-RAPID instrument. The purity of novel compounds was also determined to be >95% by elemental analysis.
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