反応 #46174

ord-3b200dad4b06471d9b74686d147c1eb5

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The mixture was reacted for 1 hour at 70° C.
  2. 2
    洗浄washed with brine
  3. 3
    抽出The organic layer was extracted with ethyl acetate
  4. 4
    乾燥dried over anhydrous sulfonate sulfate
  5. 5
    濃縮concentrated
  6. 6
    その他the resulting residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:9)

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07741323B2uspto-grants-2010_06