Bexarotene (Targretin) is a retinoid X receptor (RXR) agonist that has applications for treatment of T cell lymphoma and proposed mechanisms of action in Alzheimer’s disease that have been the subject of recent controversy. Carbon-11 labeled bexarotene ([¹¹C-carbonyl]4-[1-(3,5,5,8,8-pentamethyltetralin-2-yl)ethenyl]benzoic acid) was synthesized using a Cu-mediated cross-coupling reaction employing an arylboronate precursor 1 and [¹¹C]carbon dioxide under atmospheric pressure in 15 ± 2% uncorrected radiochemical yield (n = 3), based on [¹¹C]CO₂. Judicious choice of solvents, catalysts, and additives, as well as precursor concentration and purity of [¹¹C]CO₂, enabled the preparation of this ¹¹C-labeled carboxylic acid. Formulated [¹¹C]bexarotene was isolated (>37 mCi) with >99% radiochemical purity in 32 min. Preliminary positron emission tomography–magnetic resonance imaging revealed rapid brain uptake in nonhuman primate in the first 75 s following intravenous administration of the radiotracer (specific activity >0.3 Ci/μmol at time of injection), followed by slow clearance (Δ = −43%) over 60 min. Modest uptake (SUV_max = 0.8) was observed in whole brain and regions with high RXR expression.