反応 #47711

ord-1bd1c3cd8d8a456992990a9283a57020

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他the solvent is removed under vacuum
  2. 2
    workup.DISSOLUTIONthe residue is dissolved in dichloromethane
  3. 3
    洗浄The dichloromethane layer is washed with 10% aqueous sodium bicarbonate (3×100 mL), water (1×100 mL) and brine
  4. 4
    乾燥The separated dichloromethane layer is dried over with magnesium sulfate
  5. 5
    ろ過filtered
  6. 6
    その他evaporated

実験手順

A solution of 2.831 g (8 mmole) 3-iodomethyl-4-iodobutyric acid in 80 mL ethanol is saturated with HCl gas at 0° C. After stirring the solution at room temperature for two days, the solvent is removed under vacuum, and the residue is dissolved in dichloromethane. The dichloromethane layer is washed with 10% aqueous sodium bicarbonate (3×100 mL), water (1×100 mL) and brine. The separated dichloromethane layer is dried over with magnesium sulfate, filtered and evaporated to give ethyl-3-iodomethyl-4-iodobutyrate.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07744853B2uspto-grants-2010_06