반응 #46174

ord-3b200dad4b06471d9b74686d147c1eb5

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The mixture was reacted for 1 hour at 70° C.
  2. 2
    세척washed with brine
  3. 3
    추출The organic layer was extracted with ethyl acetate
  4. 4
    건조dried over anhydrous sulfonate sulfate
  5. 5
    농축concentrated
  6. 6
    기타the resulting residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:9)

실험 절차

3-Phenyl-6-(3-phenylpropyloxy)-1-oxo-1H-indene-2-carboxylate ethyl ester (1.65 g, 4.0 mmol) prepared in (Step 5) of Example 1 was dissolved in methanol (160 ml) and p-toluene sulfonic acid (228 mg, 1.2 mmol) was added thereto. The mixture was reacted for 1 hour at 70° C., and then washed with brine. The organic layer was extracted with ethyl acetate, dried over anhydrous sulfonate sulfate, concentrated, and the resulting residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:9) to obtain the title compound (yield 75.3%) as a red solid.

출처

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