Apexii fticr mass spectrometer

Unless stated otherwise, all reagents and solvents were purchased from commercial suppliers, and all reactions were carried out under anhydrous conditions with argon atmosphere. Yields were calculated by HPLC chromatography or ¹H NMR spectroscopy. UV spectra were obtained using a Perkin-Elmer Lambda2 UV/vis spectrometer. NMR data were collected using either a Varian INOVA 500 (¹H 500 MHz, ¹³C 126 MHz) NMR spectrometer with a 3 mm Nalorac MDBG probe or a Varian INOVA 600 (¹H 600 MHz, ¹³C 150 MHz) NMR spectrometer equipped with a 5 mm ¹H[¹³C,¹⁵N] triple resonance cold probe with a z-axis gradient, utilizing residual solvent signals for referencing. High-resolution mass spectra (HRMS) were obtained using a Bruker (Billerica, MA) APEXII FTICR mass spectrometer equipped with an actively shielded 9.4 T superconducting magnet (Magnex Scientific Ltd., UK), an external Bruker APOLLO ESI source, and a Synrad 50W CO₂ CW laser. Supelco Discover HS (4.6 × 150 mm) and semipreparative (10 × 150 mm) C18 (5 μm) columns were used for analytical and semipreparative HPLC, respectively, as conducted on a Hitachi Elite Lachrom System equipped with a Diode Array L-2455 detector. The enantiomeric excess (ee) was calculated from the area of HPLC peak using a silica-based protein phase enantiomer separation column, RESOLVOSIL BSA-7 column, eluting with 0.1 M phosphate buffer pH 7.5, 2 % 1-propanol.

Unless stated otherwise, all reagents and solvents were purchased from commercial suppliers. Yields were calculated by HPLC chromatography or ¹H NMR spectroscopy. Circular dichroism spectra were obtained on a Jasco J720A spectropolarograph. NMR data were collected using either a Varian INOVA 500 (¹H 500 MHz, ¹³C 126 MHz) NMR spectrometer with a 3 mm Nalorac MDBG probe or a Varian INOVA 600 (¹H 600 MHz, ¹³C 150 MHz) NMR spectrometer equipped with a 5 mm ¹H[¹³C,¹⁵N] triple resonance cold probe with a z-axis gradient, utilizing residual solvent signals for referencing. High-resolution mass spectra (HRMS) were obtained using a Bruker (Billerica, MA) APEXII FTICR mass spectrometer equipped with an actively shielded 9.4 T superconducting magnet (Magnex Scientific Ltd., UK), an external Bruker APOLLO ESI source, and a Synrad 50W CO₂ CW laser. Supelco Discover HS (4.6 × 150 mm) and semipreparative (10 × 150 mm) C₁₈ (5 μm) columns were used for analytical and semipreparative HPLC, respectively, as conducted on a Hitachi Elite Lachrom System equipped with a Diode Array L-2455 detector.