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Synthesis, NMR Characterization, and a Simple Application of Lithium Borotritide
Chit Than1, Hiromi Morimoto, Hendrik Andres
1National Tritium Labelling Facility, Structural Biology Division, E. O. Lawrence Berkeley National Laboratory, One Cyclotron Road, Berkeley, California 94720 and Sandoz Pharma Ltd., Chemical Research and Development, Basle CH-4002, Switzerland.
Abstract:
LiBH(4) is a powerful and selective reagent for regiospecific reduction reactions. A simple synthesis of LiB(3)H(4) at near theoretical specific radioactivity is reported. We have treated Li(3)H synthesized from tritium gas ((3)H(2), approximately 98%) with BBr(3) to produce LiB(3)H(4) (specific activity = 4120 GBq/mmol = 110 Ci/mmol. The maximum theoretical specific activity of LiB(3)H(4) is 4252 GBq/mmol = 115.04 Ci/mmol; 1 matom of (3)H = 1063 GBq = 28.76 Ci.) The tritium labeling performance of the reagent was tested by an exemplary reduction of 2-naphthaldehyde to 2-naphthalenemethanol. LiB(3)H(4) and the reduction products were characterized by a combination of (1)H, (3)H, and (11)B NMR techniques, as appropriate.