To a reflux apparatus quickly add 7 g of phosphorus pentoxide and 27.5 g of 85% phosphoric acid followed by the addition of 37 g of potassium iodide and 13 g of tert-butyl alcohol, reflux for 1h with stirring. Stop the heating and stir for 1h, thereafter pour the solution into a separatory funnel with 50 mL of water and 50 mL of hexane. Discard the aqueous layer and wash the organic with dilute sodium bicarbonate solution until no bubbling occurs then wash with 10% sodium metabisulfite solution until the brown color is disappeared. Distil the solution and collect the fraction of 99-100 ° C, dry the product with some anhydrous magnesium sulfate and store under nitrogen gas in a freezer.
Refluxing the mixture
Washing the solution
The organic layer prior to metabisulfite washing
The pure product