反応 #46975

ord-3196d557fb8848f3bf1af18536d3e07f

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to reflux for 15 h
  2. 2
    温度After cooling
  3. 3
    その他the reaction mixture was evaporated
  4. 4
    抽出extracted by CH2Cl2
  5. 5
    乾燥The combined organic layer was dried by MgSO4
  6. 6
    濃縮concentrated
  7. 7
    その他to give a residue that
  8. 8
    その他was purified by silica gel flash column chromatography (EtOAc:n-hexane=1:2)

実験手順

To a stirred solution of 18 (2 g, 4.84 mmol), AIBN (0.08 g, 0.48 mmol), Bu3SnH (3.91 ml, 14.50 mmol) in toluene (49 ml) was heated to reflux for 15 h. After cooling, the reaction mixture was evaporated and then extracted by CH2Cl2. The combined organic layer was dried by MgSO4 and concentrated to give a residue that was purified by silica gel flash column chromatography (EtOAc:n-hexane=1:2) to give compound 19, yield 90%.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07741495B2uspto-grants-2010_06