반응 #1328397

ord-bcf2bfbcb1224dfe89f8f68f9ea1b76f

반응 방정식

O=C(O)CC(CI)CI
3-iodomethyl-4-iodobutyric acid
Cl
HCl
CCO
ethanol
CCOC(=O)CC(CI)CI
ethyl-3-iodomethyl-4-iodobutyrate

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 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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07115248B2uspto-grants-2006_10