反応 #1095108

ord-0b252585547a46fe8a2240492bf34990

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The mixture is heated
  2. 2
    温度under reflux for 4 hours
  3. 3
    温度After cooling the mixture
  4. 4
    ろ過the deposited matter is collected by filtration
  5. 5
    workup.ADDITIONThe deposited matter is added to a mixture of ethyl acetate and water, pH
  6. 6
    その他the organic layer is separated
  7. 7
    洗浄The organic layer is washed with water and saturated aqueous solution of sodium chloride
  8. 8
    乾燥dried over anhydrous magnesium sulfate
  9. 9
    workup.DISTILLATIONthe solvent is distilled off under reduced pressure

実験手順

In a mixture of 58 mL of ethanol and 6 mL of water is dissolved 6.40 g of 2-(2-benzo[b]thiophen-5-ylethoxy)-1-piperidino-1-ethanone, to which is added 1.27 g of sodium hydroxide. The mixture is heated under reflux for 4 hours. After cooling the mixture, the deposited matter is collected by filtration. The deposited matter is added to a mixture of ethyl acetate and water, pH is adjusted to 1.5 with 2 mol/L hydrochloric acid, and the organic layer is separated. The organic layer is washed with water and saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, and the solvent is distilled off under reduced pressure to obtain 3.72 g of 2-(2-benzo[b]thiophen-5-ylethoxy)-acetic acid as a colorless crystalline product.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06797726B1uspto-grants-2004_09