Reaktion #170704

ord-21e353f5bbb74667aa375cb68bd24799

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONUnder nitrogen atmosphere, an appropriate amount of amberlite IR-120 was added to the reaction solution
  2. 2
    Filtrationfiltered through Celite
  3. 3
    EinengenThe filtrate was concentrated under reduced pressure, ethyl acetate
  4. 4
    workup.ADDITIONwas added to the resulting residue
  5. 5
    Trocknenthe mixture was dried over sodium sulfate
  6. 6
    Einengenagain concentrated under reduced pressure

Vorschrift

To a solution of sodium 5-oxo-2,5-dihydrofuran-3-carboxylate (150 mg) in water (3 ml) was added 10 wt % palladium on carbon (30 mg), and the mixture was stirred for 18 hours at room temperature under one atm. of hydrogen. Under nitrogen atmosphere, an appropriate amount of amberlite IR-120 was added to the reaction solution, the mixture was stirred at room temperature for 10 minutes, and then filtered through Celite. The filtrate was concentrated under reduced pressure, ethyl acetate was added to the resulting residue, the mixture was dried over sodium sulfate, and then again concentrated under reduced pressure to give the titled compound (83 mg).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846746B2uspto-grants-2014_09