반응 #46159

ord-d6c34f8707e94405ab4916f21c8158a8

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the reaction mixture was refluxed
  2. 2
    온도by cooling
  3. 3
    기타The solution obtained
  4. 4
    여과after filtering residual solid selenium dioxide
  5. 5
    추출extracted with ether/water
  6. 6
    건조The extract was dried over anhydrous magnesium sulfate
  7. 7
    농축concentrated
  8. 8
    기타the resulting residue was purified by column chromatography

실험 절차

5,6-Methylenedioxy-3-phenyl-1H-indene-2-carboxylate ethyl ester (3 g, 9.73 mmol) was dissolved in 1,4-dioxane. Selenium dioxide (10.8 g, 97.3 mmol) was added thereto and the reaction mixture was refluxed while stirring for 1 day, followed by cooling. The solution obtained after filtering residual solid selenium dioxide was combined with 1M sodium bicarbonate, and extracted with ether/water. The extract was dried over anhydrous magnesium sulfate, concentrated, and the resulting residue was purified by column chromatography to obtain 5,6-methylenedioxy-1-oxo-3-phenyl-1H-indene-2-carboxylate ethyl ester (2.18 g, yield 70%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07741323B2uspto-grants-2010_06