Reacción #81617

ord-1385067a1d49477dbeddb28bd37bd339

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturaat reflux for 72 hours
  2. 2
    FiltraciónFilter
  3. 3
    Filtraciónthrough filter aid while at 80° C.
  4. 4
    Otroseparate the organic phase
  5. 5
    SecadoDry (MgSO4)
  6. 6
    Filtraciónfilter
  7. 7
    Otropurify by chromatography (ethyl acetate)

Procedimiento

Mix 4-(4-chloro-1-oxobutyl)-2,2-dimethylphenethyl acetate (99.5 g, 0.335 mol), α,α-diphenyl-4-piperidinemethanol (101.8 g, 0.335 mol), potassium hydrogen carbonate (83.8 g, 0.838 mol), potassium iodide (1.00 g, 0.006 mol), toluene (600 mL) and water (220 mL). Stir at reflux for 72 hours, add toluene (200 mL) and deionized water (100 mL). Filter through filter aid while at 80° C. and separate the organic phase. Dry (MgSO4), filter and purify by chromatography (ethyl acetate) to give 4-[4-[4-(hydroxydiphenylmethyl)-1-piperidinyl]-1-oxobutyl]-2,2-dimethylphenethyl acetate as an oily solid.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05618940uspto-grants-1997_04