Reaktion #679968

ord-396b3d214c004f2f911f60f01eced723

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenIt was then concentrated under reduced pressure
  2. 2
    Sonstigethe residue was purified by column chromatography
  3. 3
    Wascheneluting with 15:1 dichloromethane/methanol

Vorschrift

To a solution of 189c (2.5 g, 5.6 mmol) in methanol (25 mL) was added sodium acetate (0.56 g, 6.8 mmol) and hydroxylamine hydrochloride (0.7 g, 10 mmol). The reaction mixture was stirred for 0.5 h. It was then concentrated under reduced pressure and the residue was purified by column chromatography eluting with 15:1 dichloromethane/methanol to afford 189d(1.3 g, 71%). MS: [M+H]+ 280.3.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09238655B2uspto-grants-2016_01