Process of producing cortisone and its esters

Claim 1

IN AN IMPROVED PROCESS OF PRODUCING CORTISONE AND ITS ESTERS FROM 3A,17A-DIHYDROXY-21-BROMO PREGNANE11,20-DIONE, THE STEPS COMPRISING HEATING A HOMOGENEOUS SOLUTION OF 3A,17A-DIHYDROXY-21-BRMO PREGNANE-11,20DIONE AND TERTIARY BUTANOL AT ABOUT 65-70* C. WITH NBROMO SUCCINIMIDE IN THE PRESENCE OF ABOUT 10% OF WATER, SAID BROMINATED DIKETONE AND SAID N-BORMO SUCCINIMIDE BEING REACTED WITH EACH OTHER IN THE PROPORTION OF 1 MOL OF THE BROMO DIKETONE TO 2 MOLS OF N-BROMO SUCCINIMIDE, MAINTAINING THE TEMPERATURE OF SAID REACTION MIXTURE AT 65-70* C. UNTIL A YELLOWISH TRANSPARENT SOLUTION RESULTS, DILUTING SAID SOLUTION WITH WATER AT 65-70* C. TO CAUSE CRYSTALLIZATION OF 4,21-DIBROMO-17A-HYDROXY PREGNANE-3,11-20-TRIONE, COOLING SAID MIXTURE, FILTERING OFF THE DIBROMO COMPOUND, ADDING SAID DIBROMO COMPOUND TO A SOLUTION OF SEMICARBAZIDE IN ACETIC CONTAINING SODIUM ACETATE, MAINTAINING THE TEMPERATURE OF SAID REACTION MIXTURE AT ABOUT 45* C., PRECIPITATING THE RESULTING 3-SEMICARBAZONE OF 17A-HYDROXY-21-BROMO-$4PREGNENE-3,11,20-TRIONE BY THE ADDITION OF WATER TO THE REACTION MIXTURE, SUSPENDING SAID SEMICARBAZONE IN ACETIC ACID, ADDING TO SAID SUSPENSION A CONCENTRATED AQUEOUS SOLUTION OF PYRUVIC ACID, HEATING THE MIXTURE TO 90-95* C. TO CAUSE CLEAVING OF SAID SEMICARBAZONE, COOLING THE REACTION MIXTURE, FILTERING OFF THE RESULTING CRYSTALS OF 17A-HYDROXY-21BROMO-$4-PREGNENE-3,11,20-TRIONE, ADDING SAID TRIONE COMPOUND TO A SOLUTION OF SODIUM IODIDE IN ACETONE CONTAINING A SMALL AMOUNT OF WATER, ADDING TO SAID MIXTURE AN ALKALI ACETATE BOILING SAID MIXTURE UNDER REFLUX UNTIL THE TRIKETONE IS COMPLETELY DISSOLVED AND AN AQUEOUS LAYER SEPARATES, POURING THE REACTION MIXTURE INTO ICE WATER, FILTERING OFF THE PRECIPITATED CORTISONE ACETATE, AND WASHING AND DRYING SAID CORTISONE COMPOUND.