Reaktion #40457

ord-becf4864ac49431f98c4bd814a232da9

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationUpon filtration
  2. 2
    Sonstigethrough a pad of celite and evaporation of the methanol
  3. 3
    Sonstigea dark brown solid was obtained
  4. 4
    SonstigeThe light brown solid that precipitated out
  5. 5
    Filtrationwas collected by filtration
  6. 6
    Sonstigedried thoroughly in vacuo

Vorschrift

6-chloro-7-methoxy-8-nitro-9H-β-carboline (510 mg, 1.84 mmol) was suspended in 50 ml of methanol and 100 mg of Pd/C (10%) was added. The flask was fitted with a balloon of hydrogen and the reaction mixture was stirred overnight at RT. Upon filtration through a pad of celite and evaporation of the methanol, a dark brown solid was obtained. This residue was suspended in methanol (15 ml) and added, with vigorous stirring, to a solution of saturated NaHCO3 (100 ml). The light brown solid that precipitated out was collected by filtration and dried thoroughly in vacuo to give the desired product (512 mg, quantitative yield).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07727985B2uspto-grants-2010_06