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Deactivated silica gel (prepared as a 10% water/silica gel (v/v) slurry) was utilized to mitigate the acidity of silica gel, preventing hydrolysis of the enol-acetal
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1HNMR spectrum of (+)-24 with that of the first generation synthesis confirmed the stereochemical outcome of the methylation.
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The 4 Å molecular sieves were purchased as an activated powder (< 50 μm). Activation at 100°C for 2.5 h under atmospheric pressure proved optimal.
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The 4 Å molecular sieves were purchased as an activated powder (< 50 μm). Activation at 100°C for 2.5 h under atmospheric pressure proved optimal.
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