反応 #46155

ord-770b7d6d1da4405690083fcd544e2270

反応条件

温度
70°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄washed with saturated ammonium chloride
  2. 2
    その他The organic layer obtained
  3. 3
    抽出by extracting the reaction mixture with ethyl acetate
  4. 4
    乾燥was dried over anhydrous magnesium sulfate
  5. 5
    濃縮concentrated
  6. 6
    その他the residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:2)

実験手順

3-Phenyl-6-(3-phenylpropyloxy)-1-oxo-1H-indene-2-carboxylate ethyl ester (2 g, 4.85 mmol) and hydroxyamine.hydrochloric acid (1.01 g, 14.6 mmol) were dissolved in pyridine (1.57 ml, 19.4 mmol). The reaction mixture was stirred for 1 hour at 70° C., and washed with saturated ammonium chloride. The organic layer obtained by extracting the reaction mixture with ethyl acetate was dried over anhydrous magnesium sulfate, concentrated, and the residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:2) to obtain 1-hydroxyimino-3-phenyl-6-(3-phenylpropyloxy)-1H-indene-2-carboxylate ethyl ester (yield 9.5%) as a yellow solid.

出典

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