A glucuronide of a novel cholesterol absorption inhibitor was synthesized on a 200-mg scale in one step via bovine liver glucuronyltransferase-catalyzed coupling of the glucuronyl moiety of UDP-glucuronic acid with the phenolic hydroxyl of Sch 58235. It was shown that the product yield is limited by the hydrolysis of UDP-glucuronic acid by impurities present in the commercial microsomal preparation of the transferase. This detrimental effect of UDPGluA hydrolysis could be diminished by the presence of high concentration of glucuronlytransferase. Optimization of reaction conditions and purification procedure resulted in a process that proceeded with 95% conversion and 88% isolated product yield. The C-13(6)-glucuronide of Sch 58235 was prepared with the help of a cascade of eight enzymes operating concurrently in one pot.