Reaktion #171003

ord-0b7bff0aaffd4e05ae39790fa3fd5402

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe catalyst was removed by filtration, and methanol
  2. 2
    workup.DISTILLATIONdistilled off
  3. 3
    SonstigeCrude 62 was purified by column chromatography on silica gel

Vorschrift

6-[4-(6-Benzyloxyhexanoylamino)-phenoxy]-hexanoic acid methyl ester 61 (10 g, 22.67 mmol) was dissolved in methanol (100 ml) in a pressure vessel. Palladium on carbon (5%, 6 grm) was added and the mixture stirred under a hydrogen atmosphere (4 kg) for 20 hrs. The catalyst was removed by filtration, and methanol distilled off. Crude 62 was purified by column chromatography on silica gel using chloroform as eluant to give pure 62 (5 g, 62.8%) as a white powder with a m.p. between 73-75.5° C.

Quelle

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