A one‐pot synthesis of [11C] labeled tamoxifen has been developed via reductive carboxylation. In this approach, [11C]CO2 is reacted with the N‐trimethylsilyl derivative of desmethyltamoxifen, followed by in situ sodium bis (2‐methoxyethoxy)aluminum hydride reduction, to afford impure [11C] labeled tamoxifen, which, on purification over a basic alumina‐silica gel column, provided pure [11C] tamoxifen in excellent radiochemical yield (65% to 84%) and radiochemical purity (>99%). The specific activity of [11C]tamoxifen was 250–400 Ci/mmol at the end of bombardment.