Reaktion #73713

ord-4fb7fca05294429b807745a8602b9214

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added
  2. 2
    SonstigeThe organic layer was separated
  3. 3
    Waschenthe aqueous layer was washed by 2×50 mL of diethyl ether
  4. 4
    ExtraktionThe combined organic extract
  5. 5
    Sonstigewas evaporated to dryness
  6. 6
    SonstigeThe product was isolated by flash-chromatography on silica gel 60 (40-63 um, eluent: from hexanes to hexanes-diethyl ether, 20:1, vol.)

Vorschrift

To a suspension of 0.34 g (8.0 mmol) of LiAlH4 in 25 mL of THF, 1.19 g (2.50 mmol) of 35 was added. The obtained mixture was stirred for 4 hr, and then a saturated aqueous solution of Na2SO4 was added. The organic layer was separated, and the aqueous layer was washed by 2×50 mL of diethyl ether. The combined organic extract was evaporated to dryness. The product was isolated by flash-chromatography on silica gel 60 (40-63 um, eluent: from hexanes to hexanes-diethyl ether, 20:1, vol.) to yield 0.77 g (64%) of the title product.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08541521B2uspto-grants-2013_09