Reacción #660210

ord-4b2220a64d72410ba99bbe69369cf75f

Disolventes

Condiciones de reacción

Temperatura
80°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.STIRRINGthe mixture was stirred overnight
  2. 2
    OtroAfter completion of the reaction
  3. 3
    Temperaturathe reaction mixture was cooled to room temperature
  4. 4
    Otroin a water bath to allow
  5. 5
    Otroprecipitation
  6. 6
    FiltraciónThe crystals were collected by filtration and slurry
  7. 7
    Lavadowashed once with 1N hydrochloric acid (40 ml), once with pure water (40 ml) and once with methanol (40 ml)

Procedimiento

2,7-Dihydroxy-9-fluorenone (1 g, 4.71 mmol) was dissolved in DMF (40 ml), and potassium carbonate (1.95 g, 14.1 mmol) and docosyl bromide (96%, 4.02 g, 9.91 mmol) were added. The mixture was stirred overnight at 80° C., docosyl bromide (0.40 g, 0.99 mmol) was further added and the mixture was stirred overnight. After completion of the reaction, the reaction mixture was cooled to room temperature, 1N hydrochloric acid (120 ml) was added thereto in a water bath to allow precipitation. The crystals were collected by filtration and slurry washed once with 1N hydrochloric acid (40 ml), once with pure water (40 ml) and once with methanol (40 ml) to give 2,7-didocosyloxy-9-fluorenone (4.20 g, docosyl bromide mixture).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US09029504B2uspto-grants-2015_05