379
residue was dissolved in 1 N sodium hydroxide solution
(50 mL) and tert-butyl methyl ether (50 mL). The phases
were separated. The aqueous phase was extracted with
tert-butyl methyl ether (3 × 50 mL). The combined
organic layers were dried over magnesium sulfate. The
solvent was removed in vacuo. The crude product was
purified by flash chromatography on silica (35 g), using
ethyl acetate/heptane/triethylamine (20:10:1) as eluent, to
give 99 mg of silyl ether 63.
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We thank P. Andersen, H. Christensen, K. Frandsen,
N. Birkebæk Hammerum, N. Hansen, A. Heerwagen, S.
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