【正文】
冰鹽水冷卻至 5~ 7 ℃ ,投入預(yù)先配置的 氧化劑 ,反應(yīng)罐內(nèi)溫度急劇上升,在 60~70 ℃ 保溫反應(yīng) 20min,加熱到90~100 ℃ , 常壓蒸餾 回收醋酸,再改 減壓回收醋酸到一定體積,冷卻后,加水稀釋。 OA c OO A cOC OO A cO( 3)水解- 1,4消除 在 酸性質(zhì)子的作用下 , C- 20酮發(fā)生 烯醇化 ,當其回復(fù)為酮時,則發(fā)生消除。 10 OOOHC OC H2O HO HOHOC OA c OC H3C OOHC H3OC OOC H3OC OOC H3O HBrC OOC H3O HC OOC H2IO HC OOC H2O A cO HC OOC H3OOHC OOC H3OOC OOC H3OBrO HC OOC H3OO HC OOC H2IOO HC OOC H2O A cOO HH2N C N H NC H2O A cOO HN N H C N H2OOH2N C N H NC H2O A cO HN N H C N H2OHOO犁頭霉菌 黑根霉菌 工藝路線 11 OOOHC OC H2O HO HOHOC OA c OC H3C OOHC H3OC OOC H3OC OOC H3O HBrC OOC H3O HC OOC H2IO HC OOC H2O A cO HC OOC H3OOHC OOC H3OOC OOC H3OBrO HC OOC H3OO HC OOC H2IOO HC OOC H2O A cOO HH2N C N H NC H2O A cOO HN N H C N H2OOH2N C N H NC H2O A cO HN N H C N H2OHOOOOOHC OC H2O HO HOHOC OA c OC H3C OOHC H3OC OOC H3OC OOC H3O HBrC OOC H3O HC OOC H2IO HC OOC H2O A cO HC OOC H3OOHC OOC H3OOC OOC H3OBrO HC OOC H3OO HC OOC H2IO O HC OOC H2O A cO O HH2N C N H NC H2O A cO O HN N H C N H2OOH2N C N H NC H2O A cO HN N H C N H2OHOO黑根霉菌氧化 溴代 脫溴 碘化 置換 梨頭霉菌氧化 醋酸化 合物 S 12 ? 一、合成路線 ? (一)經(jīng)醋酸可的松的合成路線 OOOHC OC H2O HO HOHOC OA c OC H3C OOHC H3OC OOC H3OC OOC H3O HBrC OOC H3O HC OOC H2IO HC OOC H2O A cO HC OOC H3OOHC OOC H3OOC OOC H3OBrO HC OOC H3OO HC OOC H2IOO HC OOC H2O A cOO HH2N C N H NC H2O A cOO HN N H C N H2OOH2N C N H NC H2O A cO HN N H C N H2OHOOOOOHC OC H2O HO HOHOC OA c OC H3C OOHC H3OC OOC H3OC OOC H3O HBrC OOC H3O HC OOC H2IO HC OOC H2O A cO HC OOC H3OOHC OOC H3OOC OOC H3OBrO HC OOC H3O O HC OOC H2IO O HC OOC H2O A cO O HH2N C N H NC H2O A cO O HN N H C N H2OOH2N C N H NC H2O A cO HN N H C N H2OHOOOOOHC OC H2O HO HOHOC OA c OC H3C OOHC H3OC OOC H3OC OOC H3O HBrC OOC H3O HC OOC H2IO HC OOC H2O A cO HC OOC H3OOHC OOC H3OOC OOC H3OBrO HC OOC H3OO HC OOC H2IOO HC OOC H2O A cOO HH2N C N H NC H2O A cOO HN N H C N H2OOH2N C N H NC H2O A cO HN N H C N H2OHOO13 OOOHC OC H2O HO HOHOC OA c OC H3C OOHC H3OC OOC H3OC OOC H3O HBrC OOC H3O HC OOC H2IO HC OOC H2O A cO HC OOC H