반응 #46974

ord-ae54213838fd4403b8d5766190111df7

반응 조건

온도
100°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도After cooling
  2. 2
    여과the reaction mixture was filtrated
  3. 3
    추출extracted with CH2Cl2
  4. 4
    건조The combined organic layer was dried by MgSO4
  5. 5
    기타evaporated
  6. 6
    기타to give a residue that
  7. 7
    기타was purified by silica gel flash column chromatography (EtOAc:n-hexane=2:3)

실험 절차

A mixture of 17 (9 g, 0.021 mol), iron (3.65 g, 0.065 mol), and ammonium chloride (2.33 g, 0.043 mol) in isopropanol (200 ml)-water (50 ml) was stirred at 100° C. for 4 h. After cooling, the reaction mixture was filtrated and extracted with CH2Cl2. The combined organic layer was dried by MgSO4 and evaporated to give a residue that was purified by silica gel flash column chromatography (EtOAc:n-hexane=2:3) to afford compound 18, yield 89%.

출처

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