t-Butyl azidoformate (CAS NO.: ), which is known as azidic acid, 1,1-dimethylethyl ester, could be produced through the following synthetic route.

In a 1-l. round-bottomed flask fitted with a mechanical stirrer are placed 82 g. (0.62 mole) of t-butyl carbazate,2 72 g. of glacial acetic acid, and 100 ml. of water. The solution is cooled in an ice bath, and 47.0 g. (0.68 mole) of solid sodium nitrite is added over a period of 40–50 minutes, the temperature being kept at 10–15°. The mixture is allowed to stand in the ice bath for 30 minutes, 100 ml. of water is added, and the floating oil is extracted into four 40-ml. portions of ether. The combined ether extracts are washed twice with 50-ml. portions of water and with 40-ml. portions of 1M sodium bicarbonate solution until no longer acidic (about three washings are required). The solution is dried over magnesium sulfate, and the ether is removed by distillation from a water bath maintained at 40–45°; water aspirator pressure of 140–150 mm. is used. The pressure is then lowered to 70 mm., and the water bath temperature is raised to 90–95°. The azide is distilled using a Claisen flask and is collected at 73–74° (70 mm.), n²⁴D 1.4227, after a few drops of fore-run. The yield is 57–72.8 g. (64–82%).