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SUMMARY I-[ 'C]-Hexobarbital was synthetized by methylation of nor-' CH3I. The maximum radiochemical yield after hexobarbital using purification by hplc is 4 7 % at a specific activity of 1.0 mCi/pmole. Synthesis time including purification is 37 min. The tissue distribution was determined in mice at different times after i.v. injection. The main accumulation of activity during the first hour after i.v. injection is in liver and kidneys. Other well perfused organs like brain, heart and lung show significant accumulation only during the first minutes after injection.