Reaktion #993675

ord-2356da8845564dd7ae3b76657b4ce586

Lösungsmittel

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe reaction medium is filtered
  2. 2
    Sonstigethe filtrate is evaporated
  3. 3
    Waschenthe organic phase is washed with water
  4. 4
    Sonstigedried
  5. 5
    Sonstigeevaporated

Vorschrift

450 mg of 3-(3-cyanophenyl)-1,6-dimethyl-1,9-dihydro-2H-pyrido[2,3-b]indol-2-one, 10 ml of AcOH, 20 ml of pyridine, 2.6 g of sodium hypophosphite and 434 mg of Raney Ni are mixed and then the mixture is heated at 60° C. for 4 hours. The reaction medium is filtered and the filtrate is evaporated; the residue is taken up in 50 ml of AcOEt/CH2Cl2 (1/1; v/v) and the organic phase is washed with water, dried and evaporated to produce the expected compound, M.p.=280° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08012991B2uspto-grants-2011_09