Optical rotations
were measured with a JASCO DIP-370 digital polarimeter.
UV and IR spectra were recorded with a JASCO V-560 and a
JASCO FT/IR-410K spectrometer, respectively. 1H and 13C
NMR spectra were recorded in ppm (ä) in CD3OD or acetoned6
with TMS as the internal standard, employing Varian Unity
plus 500 and Varian Gemini 300 spectrometers operating at
500 and 300 MHz for 1H and 125 and 75 MHz for 13C. Positive
FABMS were recorded using a JEOL JMS DX-303 spectrometer,
with glycerol as the matrix. Column chromatography was
performed with MCI gel CHP 20P (75-150 ím, Mitsubishi
Chemical Industries, Ltd.), Chromatorex ODS (Fuji Silysia),
Sephadex LH-20, and silica gel 60 (0.040-0.063 mm, 0.063-
0.200 mm, Merck). Medium-pressure liquid chromatography
(MPLC) was carried out with a prepacked column, C18-20,
equipped with a JASCO PU-986 preparative pump. TLC was
performed on precoated silica gel 60 F254 plates (0.2 mm thick,
Merck) with CHCl3-MeOH-H2O (8:2:0.1 or 7:3:0.5 v/v) or
C6H6-HCOOEt-HCOOH (1:7:1 v/v), and spots were detected
by UV illumination and by spraying with 10% H2SO4 followed
by heating, or by spraying with 2% ethanolic FeCl3 reagent.