Reaktion #615164

ord-e319c8107bad4da9832d6a0f287dc789

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethen quenched with 1M HCl (1 mL)
  2. 2
    Sonstigepartitioned between DCM
  3. 3
    Waschenlayer was washed with water and brine
  4. 4
    Trocknendried over MgSO4
  5. 5
    Sonstigepurified by CC (EA/MeOH 19:1 to 9:1 containing 1% NH4OH)
  6. 6
    Sonstigeaffording a colourless solid (26 mg; 78% yield)

Vorschrift

A solution of the compound of Example 48 (33 mg) in MeOH/DCE (5 mL; 4:1) was treated with NaBH4 (3 mg) for 30 min then quenched with 1M HCl (1 mL) and partitioned between DCM and an aq. NH4OH solution. The org. layer was washed with water and brine, dried over MgSO4 and purified by CC (EA/MeOH 19:1 to 9:1 containing 1% NH4OH) affording a colourless solid (26 mg; 78% yield).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09346804B2uspto-grants-2016_05