Reaktion #1898148

ord-8b8d07f68af74df58478088be04b392d

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe flask was evacuated
  2. 2
    workup.ADDITIONrefilled with argon three times
  3. 3
    FiltrationThe mixture is filtered through a pad of diatomaceous earth
  4. 4
    Einengenconcentrated under reduced pressure

Vorschrift

A round bottom flask is charged with 5% platinum sulfide on carbon (0.20 g, 0.039 mmol). The flask was evacuated and refilled with argon three times. To the flask is added 4-(5-chloro-3-nitro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester (2.80 g, 8.17 mmol) as a solution in a 1:1 mixture of ethyl acetate:methanol (100 mL). The mixture is placed under an atmosphere of hydrogen and stirred overnight at room temperature. The mixture is filtered through a pad of diatomaceous earth and concentrated under reduced pressure to provide 2.0 g of 4-(3-amino-5-chloro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester as a dark solid in 80% yield.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08362249B2uspto-grants-2013_01