The relaxation times of the carbon centers of virescenoside A and B, glycoside metabolites of the mushroom Oospora virescens (Link) Wallr., have been determined for different deuteriochloroform-methanol solvent mixtures. In the absence of methanol the 13C NMR spectra show broad lines, corresponding to long correlation times and the presence of hydrogenbonded intermolecular complexes. The methyl groups show a relationship between relaxation time and steric constraint, and the vinyl side chain reveals a connection of the T\ values of its two carbons with its unique geometry.
1 *,2 R *)-1-Methy l-2-[ 1-(tert -butyldimethylsiloxy )-2-(J?)-buten-3-yl]-3-cyclohexene-l-carbaldehyde (36). A solution of 30a (320 mg, 1.65 mmol) in dry DMF (1 mL) was treated with tert-butyldimethylsilyl chloride (273 mg, 1.81 mmol) and imidazole (283 mg, 4.16 mmol) at room temperature. After 5 min, the solution was diluted with ether (10 mL), washed with aqueous ammonium chloride and brine, dried, and concentrated. The residue was subjected to chromatography (silica gel, 2 g; elution
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