Ft ir 620 spectrometer

Melting points (mp) were measured using the Yanaco melting point apparatus MP-S3 and were uncorrected. Optical rotations were measured with a JASCO P-1030 polarimeter. IR spectra were recorded with a JASCO FT-IR/620 spectrometer. Single crystal X-ray diffraction was recorded using a MacScience Co., Ltd DIP 2020 Image Plate. ¹H and ¹³C NMR spectra were recorded on a Bruker Biospin AVANCE III HD 400 (400 MHz for ¹H, 100 MHz for ¹³C) and a Bruker Biospin AVANCE III HD 500 (500 MHz for ¹H, 125 MHz for ¹³C). The reported chemical shifts (δ) in parts per million (ppm) were relative to the internal CHCl₃ (7.26 ppm for ¹H and 77.0 ppm for ¹³C); the coupling constant (J) values were measured in hertz. The coupling patterns are denoted as s (singlet), d (doublet), t (triplet), q (quartet), m (multiplet), and br (broad). HR-ESI-MS spectra were obtained using a Micromass LCT spectrometer with a time-of-flight (TOF) analyzer. Elemental analysis data were obtained using an Elementar Vario EL. Precoated silica gel plates with a fluorescent indicator (Merck 60 F254) were used for analytical and preparative thin-layer chromatography (TLC). Flash column chromatography was performed using Kanto Chemical silica gel 60N (spherical, natural) 40–50 μm. All reagents (Aldrich, Kanto, TCI, and Wako) and solvents were of commercial quality and were used as received.