Reaktion #73067

ord-4b5d7e18757e41bbb1458619541cc732

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigefor 55 hours
  2. 2
    FiltrationThe reaction mixture was filtered through a layer of CELITE
  3. 3
    Filtrationfilter aid
  4. 4
    Waschenthe filter cake was rinsed with methanol (100 mL)
  5. 5
    EinengenThe filtrate was concentrated under reduced pressure

Vorschrift

Palladium hydroxide (2.3 g of 20% on carbon) was added to a solution of 1-methyl-4-nitromethylpiperidin-4-ol (11.57 g) in ethanol (120 mL). The mixture was placed under hydrogen pressure (50 psi, 3.4×105 Pa) on a Parr apparatus for 55 hours. The reaction mixture was filtered through a layer of CELITE filter aid and the filter cake was rinsed with methanol (100 mL). The filtrate was concentrated under reduced pressure to provide 10.18 g of 4-aminomethyl-1-methylpiperidin-4-ol as a thick oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08541438B2uspto-grants-2013_09