反应 #46155

ord-770b7d6d1da4405690083fcd544e2270

反应条件

温度
70°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤washed with saturated ammonium chloride
  2. 2
    其他The organic layer obtained
  3. 3
    萃取by extracting the reaction mixture with ethyl acetate
  4. 4
    干燥was dried over anhydrous magnesium sulfate
  5. 5
    浓缩concentrated
  6. 6
    其他the residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:2)

实验过程

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.

来源

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