반응 #46975

ord-3196d557fb8848f3bf1af18536d3e07f

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도to reflux for 15 h
  2. 2
    온도After cooling
  3. 3
    기타the reaction mixture was evaporated
  4. 4
    추출extracted by CH2Cl2
  5. 5
    건조The combined organic layer was dried by MgSO4
  6. 6
    농축concentrated
  7. 7
    기타to give a residue that
  8. 8
    기타was purified by silica gel flash column chromatography (EtOAc:n-hexane=1:2)

실험 절차

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%.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07741495B2uspto-grants-2010_06