Reaktion #47837

ord-57f58d076584492c981c33d3ab69813d

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeat 0° C
  2. 2
    Waschenwashed with saturated saline
  3. 3
    Extraktionextracted with dichloromethane
  4. 4
    SonstigeThe organic layer was separated
  5. 5
    Trocknendried over anhydrous MgSO4
  6. 6
    Einengenconcentrated under a reduced pressure
  7. 7
    SonstigeThe resulting residue was purified by flash chromatography

Vorschrift

1-Amino-6-methoxy-3-phenyl-1H-indene-2-carboxylic acid ethyl ester (60 mg, 0.19 mmol) prepared in Example 20 was dissolved in dichloromethane (10 mL), and acetyl chloride (76.15 mg, 70.0 μl, 0.97 mmol) and triethylamine (130.00 mg, 0.18 mL, 128 mmol) were added thereto in order at 0° C. The mixture was stirred for 1 hr at RT, washed with saturated saline and extracted with dichloromethane. The organic layer was separated, dried over anhydrous MgSO4 and concentrated under a reduced pressure. The resulting residue was purified by flash chromatography to obtain 48 mg of the titled compound (yield: 71%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07745439B2uspto-grants-2010_06