Spdm20a vp diode photodiode array detector

Optical rotations were measured on a Jasco-DIP-700 polarimeter at the sodium line (589 nm). UV spectra were obtained on a Hewlett-Packard 8453 spectrophotometer and IR spectra were measured as a thin film on a CaF₂ disc using a Perkin Elmer 1600 series FTIR. ECD measurements were obtained on a Chirascan Circular Dichroism Spectrometer with the samples dissolved in MeOH and placed in a 1 cm quartz cuvette with a solvent subtraction for baseline correction. NMR spectra were acquired on a Varian Inova Unity 500 MHz spectrometer operating at 500 (¹H) or 125 (¹³C) MHz using the residual solvent signals as an internal reference. Samples were in 3 mm Shigemi tubes during NMR analyses. High-resolution mass spectrometry data were obtained on an Agilent LC-TOF or LC-QTOF with ES ionization. Gradient separations used a Shimadzu system consisting of LC-20AT Solvent Delivery Modules, an SPD-M20A VP Diode Photodiode Array Detector, and a SCL-20A VP System Controller. TLC analyses were performed on Si₆₀F₂₅₄ plates and visualized under UV or by heating after spraying with a 1% anisaldehyde solution in acetic acid:H₂SO₄ (50:1). Samples were weighted on a Mettler Toledo analytical balance.