Reaktion #589051

ord-292e16187f924a95b9a0a705b3ed5f3e

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: US07772352B2uspto-grants-2010_08