Deuterio-Raney nickel catalyst

Clean sodium (0.19 g), free of paraffin or petroleum residues, is dissolved in deuterium oxide (1.2 ml) and Raney nickel alloy (0.25 g) is added in small portions over 8 min while maintaining the temperature at about 50°. When the addition is complete, the supernatant is poured off and the catalyst is washed by decantation with deuterium oxide (3x2 ml) followed by methanol-OD (2x1 ml). The catalyst should be prepared fresh as needed and the preparation carried out as rapidly as possible. 

An alternative preparation of deuterio-Raney nickel is described using a more elaborate purification procedure. There is no evidence however, that the use of this nickel results in a better yield or higher isotopic purity of products from the desulfurization reactions. 

Audier, S. Bory, G. Defaye, M. Fetizon and G. Moreau, Bull. Soc. Chim. France, 1966, 3181. 

Biemann, Mass Spectrometry, McGraw-Hill Book Co., Inc., New York, 1962, Chapter 5. 

Chemistry Dept., Cornell University, personal communications. 

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