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A mixture of steroid (1 mmol), acetic anhydride (2.0–
3.0 mmol per hydroxyl group to be acetylated, and
6–12 mmol for enol acetylation) and toluene-p-sulfonic
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individual steroids) in a beaker or test tube was subjected to
the continuous mode of microwave irradiation (925 W) at
high power setting in a domestic type microwave oven. The
desired parameter (microwave power and time) for enol
acetylation of carbonyl group or complete acetylation of
hydroxyl groups were set as reported in the respective
tables. After completion of the reaction (checked by TLC),
the contents were brought to room temperature, mixed with
ice and water and stirred until product fell out. The solid was
filtered under suction, washed with saturated sodium
bicarbonate solution followed by water. The dried material
was used as such for purity and composition analyses by
LC-MS (see Table for details).
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Acknowledgements
This work was supported by Hollis Eden Pharmaceuticals,
San Diego, CA, USA.
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