반응 #45821

ord-4e81da8c260d410aa8bfa1025a4fbfe9

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The reaction liquid
  2. 2
    농축was concentrated under reduced pressure
  3. 3
    workup.ADDITION1 N hydrochloric acid (100 ml) and water (100 ml) were added
  4. 4
    추출the product was extracted with ethyl acetate (200 ml×2)
  5. 5
    세척The organic layer was washed with saturated brine (50 ml×2)
  6. 6
    건조dried over anhydrous magnesium sulfate
  7. 7
    농축concentrated under reduced pressure

실험 절차

A methanol (12 ml) solution of potassium hydroxide (1.26 g, 22.5 mol) was put into a tetrahydrofuran (50 ml) solution of methyl 4-bromo-2-tert-butyl-5-phenyl-1-benzofuran-7-carboxylate (I-255) (2.90 g, 7.49 mmol), followed by stirring at room temperature for 3.5 hours. The reaction liquid was concentrated under reduced pressure, then 1 N hydrochloric acid (100 ml) and water (100 ml) were added, the product was extracted with ethyl acetate (200 ml×2). The organic layer was washed with saturated brine (50 ml×2), then dried over anhydrous magnesium sulfate, concentrated under reduced pressure to obtain the entitled compound (2.64 g, 95%) as a yellow white solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07737166B2uspto-grants-2010_06