P 2300

Melting points were measured on a Yanagimoto micro apparatus without correction. Measurement of optical rotation was carried out on a JASCO P-2300 in CHCl3 solution at 23 °C. IR spectra were recorded using a Perkin-Elmer Model Spectrum 100. ¹H (400 or 600 MHz)- and ¹³C (100 or 150 MHz)-NMR spectra were recorded on a JEOL AL-400 or ECA-600 spectrometer using tetramethylsilane as an internal standard. The chemical shifts are expressed on the δ scale. EI-MS and HREI-MS were measured at 30–60 eV (direct inlet) with a JEOL Model JMS-700 and the relative intensities of peaks are reported with reference to the most intense peak higher than m/z 100. TLC was carried out on pre-coated silica gel 60 (Merck 5554) with n-hexane-EtOAc or CHCl₃-MeOH as the developing phase. Detection was carried out by spraying with concentrated H2SO₄ followed by heating. HPLC was performed on a Hitachi L-6000 equipped with a Hitachi L-7490 RI detector. The following column and solvents were used for elution: Mightysil, RP-18 GP 250–10 (25 cm x 10 mm i.d., 5μm) with MeOH-H₂O or CH₃CN-H₂O.