A rapid and easily performed procedure for the synthesis of 5β-cholestane-3α, 7β, 12α, 25- tetrol by means of an efficient homologation sequence of the intermediate, 3α, 7β, 12α- triformyloxy-24-oxo-25-diazo-25-homo-5β-cholane is described. The reaction sequence involved treating the intermediate, α-diazoketone in methanol with 3% AgNO3 or Ag2O, anhydrous Na2CO3, Na 2S 2O 3H 2O resulting in the formation of homoursocholic acid in ...