Reaktion #62377

ord-06e895fce5144a5ca92846444e67f562

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGstirred at room temperature for 10 minutes
  2. 2
    Sonstigethe reaction
  3. 3
    ExtraktionAfter extracting the aqueous phase with ethyl acetate
  4. 4
    Waschenthe organic phase was washed with water and saturated brine
  5. 5
    Trocknendried over anhydrous magnesium sulfate
  6. 6
    SonstigeThe solvent was evaporated

Vorschrift

170 mg of furan-2,5-dicarboxylic acid monobenzyl ester was dissolved in 5 mL of tetrahydrofuran, and added with 144 μl of triethylamine. After cooling to 0° C., 72.3 μl of ethyl chloroformate was added dropwise and stirred at this temperature for 30 minutes. 1 mL of concentrated ammonia water was added and stirred at room temperature for 10 minutes, and then aqueous ammonium chloride was added to stop the reaction. After extracting the aqueous phase with ethyl acetate, the organic phase was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated, to afford 185 mg of the title compound as white crystals.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07429609B2uspto-grants-2008_09