Reaktion #171002

ord-c01af6c225694f85a1ba115dce5f7d20

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeCatalyst was removed by filtration and methanol
  2. 2
    workup.DISTILLATIONdistilled off
  3. 3
    SonstigeCrude 60 was purified by column chromatography on silica gel

Vorschrift

2-[4-(6-Benzyloxyhexanoylamino)-phenoxy]-propionic acid methyl ester 59 (15 g, 37.59 mmol) was dissolved in methanol (150 ml) in a pressure vessel. Palladium on carbon (50% wet, 5%, 15 g) was added and the mixture stirred under hydrogen atmos-phere (4 kg) for 16 hrs. Catalyst was removed by filtration and methanol distilled off. Crude 60 was purified by column chromatography on silica gel using chloroform as eluant to get pure 60 (6 g, 51.6%) as a white powder with an m.p between 62-64.5° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846845B2uspto-grants-2014_09