반응 #464319

ord-d9ee218ebf4c4edcbb3f20ca6b21305e

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the solvent is removed under vacuum
  2. 2
    workup.DISSOLUTIONthe residue is dissolved in dichloromethane
  3. 3
    세척The dichloromethane layer is washed with 10% aqueous sodium bicarbonate (3×100 mL), water (1×100 mL) and brine
  4. 4
    건조The separated dichloromethane layer is dried over with magnesium sulfate
  5. 5
    여과filtered
  6. 6
    기타evaporated

실험 절차

A solution of 2.831 g (8 mmole) 3-iodomethyl-4-iodobutyric acid 17 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 18.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06024937uspto-grants-2000_02