Reaktion #79791

ord-46378615f60640858a0eda9cafb3fe72

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigewas passed through for 1 minute
  2. 2
    SonstigeThe flask was capped
  3. 3
    Sonstigeprecipitate formed
  4. 4
    FiltrationThe solid was collected by filtration

Vorschrift

3-[4-Amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]cyclopentyl 2-[(tert-butoxycarbonyl)amino]acetate (39 mg, 0.072 mmol) was dissolved in ethyl acetate (2.5 ml). Hydrogen chloride gas was passed through for 1 minute. The flask was capped and the solution stirred for additional 30 minutes. Diethyl ether was added and precipitate formed. The solid was collected by filtration to give 3-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]cyclopentyl 2-aminoacetate hydrochloride. The structure was confirmed by 1H NMR and LC/MS (MH+=444).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06713474B2uspto-grants-2004_03