Dess-Martin Periodnane (DMP)
In a wide-mouth flask with a large stirbar, a mixture of TsOH.monohydrate 0.5g and acetic anhydride 400mL was heated on oil bath to 80C. With vigorous stirring, IBX 100g was slowly added, spoon-by-spoon with internal thermometer checking the reaction mixture temperature. (It is very important to avoid overheating – the overheated mixture can produce a violent runaway and /or explosion). After complete IBX addition the mixture was stirred at 80C for 2 hours. The stirbar was removed, the mixture was placed into a cold room (+4C) overnight. The crystallized product was collected by filtration under positive pressure of nitrogen using a large (0.5L) sintered funnel. The product was washed with anhydrous ether (200mL, in portions) under positive pressure and dried by passing nitrogen through the solid.
Y = 134.2g (88.5% th) of a white powder. The product is best stored in a fridge in a tight bottle.
This procedure is from Ireland, JOC (1993), 2899