Preparation of tritium-labelled BIIL 260 of high specific radioactivity

Various approaches to the synthesis of tritium-labelled BIIL 260 with high specific radioactivity were investigated. Attempts to incorporate tritium directly into BIIL 260 were made by solid-phase isotope exchange with tritium gas and by isotope exchange with tritiated water which yielded a final product with specific activities ranging from 2 to 7 Ci/mmol. However, the solid-phase and liquid-phase dehalogenations of an appropriate synthon fragment of BIIL 260 followed by its subsequent conversion to the final product via chemical synthesis yielded the desired tritium-labelled BIIL 260 with specific activities of 25 or 71 Ci/mmol, depending upon the precursors and methods used in the dehalogenation step. Copyright (C) 2002 John Wiley Sons, Ltd.