Reaktion #838631

ord-9f41d3e77693420ba350376fbb724d28

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter destroying the excess lithium aluminum hydride
  2. 2
    workup.ADDITIONby adding a saturated sodium sulfate solution (30 μl)
  3. 3
    Filtrationthe alumina precipitate is filtered
  4. 4
    TrocknenThe filtrate, dried (MgSO4)
  5. 5
    Sonstigeevaporated under reduced pressure

Vorschrift

To a solution of ethyl Z-2-(1-hydroxy-1-methylethyl)-3-iodoacrylate (II) (4.9 mmol, 1.4 g) in anhydrous ether (30 ml), lithium aluminum hydride (2.9 mmol, 0.112 g) is added. The reaction is stirred for 1 h under an inert atmosphere (argon) at room temperature (rt). After destroying the excess lithium aluminum hydride by adding a saturated sodium sulfate solution (30 μl), the alumina precipitate is filtered. The filtrate, dried (MgSO4) and evaporated under reduced pressure, gives a white residue of E-2-(1-hydroxy-1-methylethyl)-3-iodoprop-2-en-1-ol (III) (0.9 g, 75%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07405309B2uspto-grants-2008_07