METHOD OF PREPARING D-ESTERA-1,3,5(10)TRIEN-3-OL-17-ONE (ESTRONE) Russian patent published in 2001 - IPC

FIELD: chemical industry. SUBSTANCE: method comprises, reductive aromatization of androsta-1,4-diene-3,17-dione 17- ethylene ketal by addition thereof to reaction mixture containing metallic sodium and diphenyl in diglyme at elevated temperature followed by acid hydrolysis, androsta 1,4-diene, 3,17-diene 17-ethylene ketal being added to reaction mixture in the from of solution in diphenyl melt in current of inert gas. Reaction mixture comprises amount of diphenyl which is less than stoichiometric amount, and remaining amount of diphenyl required for conducting reaction is added by addition of androsta-1,4 diene, 3,17- dione 17-ethylene ketal in melted diphenyl. Solution of androsta-1,4- diene-3,17-dione 17-ethylene ketal in diphenyl melt is prepared by mixing equal amounts of androsta-1,4-diene-3,17-dione-3,17- dione 17 ethylene ketal and diphenyl at temperature of higher than 75 C. Additional amount of estrone that remained in mother liquor after recovery of main amount is isolated by extraction with aqueous solution of sodium hydroxide, 20-40 % solution of sodium hydroxide is used for regeneration of diglyme and diphenyl. Method makes if possible to carry out reaction uniformly, recover completely estrone and partially regenerate reagents used. EFFECT: more efficient preparation method. 6 cl, 2 ex