Reaktion #163339

ord-16669a0397984d15a494644914e4ddfe

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeafter removing of the cooling bath
  2. 2
    SonstigeThe reaction mixture is quenched in ice cold water
  3. 3
    Extraktionextracted with EtOAc
  4. 4
    TrocknenThe organic layer is dried with Na2SO4
  5. 5
    Sonstigethe solvent is removed in vacuo
  6. 6
    SonstigeThe crude product is purified by column chromatography (silica gel, DCM/MeOH 98.5/1.5)

Vorschrift

3.00 g (12.1 mmol) 4-iodophenethylamine and 0.37 g (3.03 mmol) DMAP in 50 mL THF are cooled down to 0° C. 4.95 g (48.5 mmol) acetic anhydride are added and, after removing of the cooling bath, the reaction mixture is stirred for 5 h at r.t. The reaction mixture is quenched in ice cold water and extracted with EtOAc. The organic layer is dried with Na2SO4 and the solvent is removed in vacuo. The crude product is purified by column chromatography (silica gel, DCM/MeOH 98.5/1.5).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08835472B2uspto-grants-2014_09