Reaktion #72716

ord-4a9fdad254f04dc1b4dd32db485b3fe6

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled again
  2. 2
    ExtraktionExtraction of the aqueous solution
  3. 3
    TrocknenThen, the combined organic layers were dried over MgSO4
  4. 4
    Sonstigethe solvent was removed by reduced pressure
  5. 5
    SonstigeThe residue was triturated
  6. 6
    Filtrationthe product was collected by filtration in 80% yield

Vorschrift

To a stirred solution of glycine (100 mmol) and NaOH (100 mmol) in water (300 ml), at 5° C., o-chloro-benzoyl chloride (110 mmol) was added in small portions. The reaction mixture was stirred for 30 minutes at room temperature, then cooled again and acidified to pH=2 by addition of 6 M HCl. Extraction of the aqueous solution was performed with EtOAc. Then, the combined organic layers were dried over MgSO4 and the solvent was removed by reduced pressure. The residue was triturated in boiling chloroform, and the product was collected by filtration in 80% yield.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08541428B2uspto-grants-2013_09