The general procedure for the synthesis of the target compound (CAS: 4134-58-1) using the compound (CAS: 83984-86-5) as starting material was as follows: the diester (51 g, melting point 192-196°C) was dissolved in a solvent mixture of 1.4 liters of technical grade xylene and 510 ml of cyclohexanone. Water was removed from the system by distillation (250 ml of distillate was collected). Subsequently, aluminum isopropoxide (51 g) dissolved in 210 ml of xylene was added dropwise to the reaction system over a period of 5 minutes under slow distillation conditions, and distillation was continued for 45 minutes (another 210 ml of distillate was collected). Upon completion of the reaction, the mixture was rapidly cooled, the reaction was quenched by the addition of an ice-water mixture, and the remaining solvent was removed by steam distillation. The resulting solid product was collected by filtration and dried. The crude product was extracted using hot acetone and subsequently recrystallized by acetone to give 40.7 g (86% yield) of 17α-acetoxy-progesterone with a melting point of 240-243 °C. The melting point of the further purified sample was raised to 243-247 °C. *The 2% yield of the raw material is equivalent to 78.95%.
