Reaktion #2012378

ord-a5b4e9a0ab3a4148ad224611bed0f1af

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeA 500 mL five-neck flask equipped with a thermometer
  2. 2
    Temperaturwas cooled in an ice bath
  3. 3
    TemperaturThe mixture was heated
  4. 4
    Sonstigeto react at 60° C. for 4 hours
  5. 5
    Filtrationan organic layer was filtered
  6. 6
    Waschenwashed by pure water and saturated sodium chloride aqueous solution
  7. 7
    workup.ADDITIONadded into methanol so as
  8. 8
    Sonstigeto separate a product
  9. 9
    SonstigeThe obtained product was dried under reduced pressure

Vorschrift

A 500 mL five-neck flask equipped with a thermometer, an agitator, a reflux tube, a nitrogen introduction tube and an exhaust tube to a trap containing 30% aqueous sodium hydroxide was cooled in an ice bath. 6.47 g (0.022 mol) of 1,3-dibromo-adamantane, 200 ml of phenol and 2.6 g (0.01 mol) of aluminum tribromide were added to the flask and agitated at 0° C. for 6 hours. The mixture was heated to react at 60° C. for 4 hours. A reactant was poured into a 2,000 L of acid iced water. After the ice was melted, an organic layer was filtered, washed by pure water and saturated sodium chloride aqueous solution, and added into methanol so as to separate a product. The obtained product was dried under reduced pressure, thus obtaining 3.5 g of the product.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08178631B2uspto-grants-2012_05