Reaktion #166409

ord-7125caf86ff74a11ba1481bce2255e20

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with DCM twice
  2. 2
    TrocknenThe combined organics were dried over Na2SO4
  3. 3
    Einengenconcentrated in vacuo

Vorschrift

To a solution of compound 397 (39.7 g, 180 mmol) in dichloromethane (350 mL) was added triethylamine (50.0 mL, 359 mmol), followed by dropwise addition of chloroacetyl chloride (16.5 mL, 207 mmol) over 15 minutes. The resulting solution was stirred at room temperature for 1.25 hours. The crude mixture was diluted with DCM and water, and extracted with DCM twice. The combined organics were dried over Na2SO4 and concentrated in vacuo to give compound 398 (41.9 g, 78%). LCMS-ESI (POS), M/Z, M+1: Found 297.1, Calculated 297.1.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08841312B2uspto-grants-2014_09