[14C]Formaldehyde was synthesized by reducing 14CO2 at ambient temperature with Schwartz's reagent. The [14C]formaldehyde was then used in the radiosynthesis of high specific activity (2.1 GBq/mmol) [14C]hydrochlorothiazide via cyclization of 4‐amino‐5‐chloro‐1,3‐benzenedisulfonamide.