Sodium periodate, alumina-supported

The sulfide 1 (0.75 mmol) is dissolved in dichloromethane (2-3 mL) and adsorbed over silica supported sodium periodate (20%, 1.36 g, 1.28 mmol) that is wetted with 0.3 mL of water by thoroughly mixing on a vortex mixture. The adsorbed powdered material is transferred to a glass test tube and is inserted in an alumina bath (alumina 100 g, mesh 65-325, Fisher scientific bath 5.7 cm diameter) inside the microwave oven. The compound is irradiated for the time specified in the table and the completion of the reaction is monitored by TLC examination. After completion of the reaction, the product is extracted into ethyl acetate (2x15 mL). The removal of solvent at reduced pressure affords crude sulfoxide 2 that contains less than 5% sulfone. The final purification is achieved by column chromatography over silica gel column or a simple crystallization. 

A second crystalline modification of similar composition, called sodium /3"-alumina, permits exchange forNa+ by metal ions and supports the rapid migration of most cations in the periodic table, including multivalent ones. Because it can serve as a single crystal or powder host for multivalent cations, sodium /3"-alumina has a variety of potential uses as a solid electrolyte and in optical and electrical devices and has excited much current interest. 

Laboratory investigation revealed that sodium, which was present in the support to the extent of several tenths of 1%, had a profound effect on stability and activity of the moiybdena-alumina catalyst. Over a period of time it was possible to alter the procedure for preparing the support on successive occasions until the catalyst contained much less than 0.1% sodium oxide. The reduction in sodium content of the support was immediately reflected in improved catalyst life. Ultimately the life was extended to 9 to 12 months before replacement. Various forms of alumina have been used as a support, including alumina gel and a stabilized alumina gel. Moiybdena-alumina catalyst has been employed exclusively in the eight commercial plants previously referred to. Today the majority of refiners who operate hydroformers are using molybdena on alumina gel as a catalyst. The molybdic oxide content of the catalyst is somewhat below 10%. Although similar to the original catalyst as far as chemical composition is concerned, it possesses superior activity and life. 

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