in this synthesis were of reagent grade or better and were inspected
and released for use based on the manufacturer’s Certificates
of Analysis. Prednisolone was from Steraloids, deuterium gas was from
Cambridge Isotopes, Wilkinson’s catalyst was from Combi-Chem,
sodium borohydride was from Oakwood, t-butanol was
from Alfa Aesar, anhydrous dioxane, toluene, dichloromethane, methanol,
and deuterated methanol were from Acros, and all remaining chemicals
and solvents were from Sigma-Aldrich. HPLC analyses used HPLC-grade
acetonitrile (Fisher), HPLC-grade ammonium acetate (Fisher), and deionized
water. For high-resolution LC–MS, water and acetonitrile were
from Fisher (Optima LC/MS grade); ammonium acetate was from Fluka
(LC–MS ultra grade).