Methanol → Exemestane

関与物質

反応条件

反応手順

6-Methylen-androst-4-ene-3,17-dione (5.0 gm) was dissolved in N-methylpyrrolidine (25 mL) at RT & to it was charged Chloranil (12.37 gm) at RT. The reaction mass was heated to 75 to 80° C. for 18 hours. The progress of the reaction is monitored on TLC. The reaction mass was cooled down to room temperature and methanol was added to it. The reaction mass was stirred for next 30 minutes and precipitated solid mass was filtered through buchner funnel and washed with methanol. All the filtrates were combined and suitably diluted. The product from aqueous solution was extracted in toluene. Combined toluene extracts was washed with 2% aqueous NaOH solution under stirring for 30 minutes. The toluene layer was separated and washed with water. Toluene layer was dried over sodium sulfate, filtered and evaporated at reduced pressure to get solid residue. The solid residue was treated with MTBE to get 3.0 gm solid product. HPLC Purity: 97%.

情報源と証拠