tert-Butyl hypochlorite (CAS NO.: ) could be produced through the following synthetic routes.

A solution of 80 g. (2 moles) of sodium hydroxide in about 500 ml. of water is prepared in a 2-l. three-necked round-bottomed flask equipped with a gas inlet tube reaching nearly to the bottom of the flask, a gas outlet tube, and a mechanical stirrer. The flask is placed in a water bath at 15–20°, and, after the contents have cooled to this temperature, 74 g. (96 ml., 1 mole) of tert-butyl alcohol is added together with enough water (about 500 ml.) to form a homogeneous solution. With constant stirring, chlorine is passed into the mixture for 30 minutes at a rate of approximately 1 l. per minute and then for an additional 30 minutes at a rate of 0.5–0.6 l. per minute.

The upper oily layer is then separated with the aid of a separatory funnel. It is washed with 50-ml. portions of 10% sodium carbonate solution until the washings are no longer acidic to . It is finally washed 4 times with an equal volume of water and dried over calcium chloride. The yield is 78–107 g. (72–99%); d₂₀20 0.910; n²⁰D 1.403. The product is best stored under an inert atmosphere in sealed bottles kept in the dark in a refrigerator.

Notice: This preparation should be carried out in a good hood. The product should be protected from strong light, over-heating, or exposure to rubber to avoid vigorous decomposition.