Reaktion #1798211

ord-2232855a4486400383432d0a3153db46

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenconcentrated to dryness
  2. 2
    Extraktionextracted with EtOAc
  3. 3
    ExtraktionThe organic extract
  4. 4
    Sonstigewas collected
  5. 5
    Trocknendried over anhydrous Na2SO4
  6. 6
    Einengenconcentrated under reduced pressure

Vorschrift

To a solution of 256 (168.4 mg, 0.478 mmol) and NiCl2×6H2O (226 mg, 0.956 mmol) in MeOH/THF (10/10 mL) NaBH4 (72 mg, 1.92 mmol) was carefully added. The reaction mixture was stirred for 10 min, concentrated to dryness and the resultant solid was suspended in 10% HCl. The aqueous solution was basified (pH ˜11) with concentrated aqueous NH4OH and extracted with EtOAc. The organic extract was collected, dried over anhydrous Na2SO4 and concentrated under reduced pressure, to afford title compound 257 (134.6 mg, 87% yield) as a white solid. MS (m/z): 322.09 (M+1).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07790729B2uspto-grants-2010_09