反応 #81468

ord-94d92c56bf574920853a00aa70205454

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他had formed
  2. 2
    ろ過The mixture was then filtered
  3. 3
    濃縮the filtrate concentrated
  4. 4
    その他to afford the crude product which
  5. 5
    その他was recrystallised firstly from ethanol/water (1:1)

実験手順

To a stirred suspension of finely powdered 17-(3-pyridyl)androsta-5,16-dien-3β-ol (3.50 g, 10 mmol) in dry diethyl ether (150 ml) coning triethylamine (2,3 ml, 16 mmol) and dimethylaminopyridine (0.012 g, 0.1 mmol) was added acetyl chloride (1.0 ml, 14 mmol). The mixture was then stirred at ambient temperature for 12 h, over which time a thick whim precipitate of triethylammonium chloride had formed. The mixture was then filtered and the filtrate concentrated to afford the crude product which was recrystallised firstly from ethanol/water (1:1), then finally from hexane to afford the title compound (3.30 g, 84%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05618807uspto-grants-1997_04