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A very efficient and environmentally benign method has been developed for the synthesis of 25-hydroxycholesterol. The reaction was performed in THF–water (4:1, v/v) using NBS as the brominating agent, followed by the easy reduction of C–Br with lithium aluminum hydride in THF, to yield the final product corresponding to a Markovnikov’s rule. Excellent yields and regioselectivity have been obtained.
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