Reaktion #52958

ord-ce27f04eb10b4ae48baafe154c63f1b2

Lösungsmittel

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    workup.STIRRINGby stirring at room temperature for 2 h
  2. 2
    SonstigeTHF was evaporated
  3. 3
    workup.ADDITIONfresh THF (5 mL) was added
  4. 4
    Sonstigethe solution was evaporated again
  5. 5
    Sonstigethe residue was dried under vacuum

Vorschrift

To a solution of N-(2,6-dichlorobenzoyl)-4-(2,6-dimethoxyphenyl)-L-phenylalanine (0.1 g) in THF (5 mL) at 0° C. under N2 was added oxalyl chloride (0.055 mL) followed by a drop of DMF. The solution was stirred at 0° C. for 2 h followed by stirring at room temperature for 2 h. THF was evaporated and fresh THF (5 mL) was added and the solution was evaporated again. This process was repeated one more time and the residue was dried under vacuum to yield N-(2,6-dichlorobenzoyl)-4-(2,6-dimethoxyphenyl)-L-phenylalanyl chloride.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06855843B2uspto-grants-2005_02