Abstract: | Abstract A method for preparing 21,21,22-2H3] digoxin by proton exchange with D2O under high temperature and basic conditions is described. Loss of signal for the protons at C21 and C22 upon deuteration, with retention of structural integrity for the remainder of the parent compound, is established with high resolution proton NMR spectroscopy. Confirmation of the site of deuterium exchange and relative abundance of the species 2H0:2H1:2H2:2H3 is demonstrated by capillary gas chromatography - mass spectrometry (GC-MS) of the trimethylsilyl derivative of the steroidal component of digoxin, digoxigenin. |