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29. Experimental
References and notes
General remarks: All reagents were obtained from commercial sources (Aldrich
Chemical Co.) and used without further purification. All solvents were of
analytical grade. All extracts were dried over anhydrous Na2SO4. 1H and 13C
NMR spectra were recorded on a Bruker AC 200 (1H NMR, 200 MHz; 13C NMR,
50.32 MHz) CDCl3 was used as the solvent and tetramethylsilane as an internal
standard. Reactions were routinely monitored by TLC using Merck silica gel
F254 plates and visualization of TLC spots with a freshly prepared 7% ethanolic
solution of phosphomolibdic acid. Silica gel 40 (0.063–0.200 mm) from Merck
was used for column chromatography. GC and GC–MS analyses were
performed on a Hewlett-Packard gas chromatograph, model 5890 equipped
with a FID detector and coupled to an electronic integrator. The chromatograph
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