Reaktion #58097

ord-b205cd67cc5f4963b841b1479888a34a

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe mixture is partitioned between DCM and saturated sodium carbonate solution
  2. 2
    SonstigeThe layer is separated
  3. 3
    Extraktionthe aqueous layer is extracted with DCM
  4. 4
    WaschenThe combined organic extracts are washed with brine
  5. 5
    Trocknendried over Na2SO4
  6. 6
    Filtrationfiltered
  7. 7
    Einengenconcentrated

Vorschrift

To a solution of 3-bromo-4-methylaniline (1.27 g, 6.82 mmol) in DCM (20 mL) at (0° C. is added acetic anhydride (0.676 mL, 7.16 mmol) dropwise. After 30 minutes, the mixture is partitioned between DCM and saturated sodium carbonate solution. The layer is separated and the aqueous layer is extracted with DCM. The combined organic extracts are washed with brine, dried over Na2SO4, filtered and concentrated to afford the title compound (1.55 g, 99%). The residue is used in the next step without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07423038B2uspto-grants-2008_09