Reaktion #2282761

ord-e07396aaff6d440da73db7ae8df03a4e

Reaktionsgleichung

[Na+].[OH-]
sodium hydroxide
Oc1ccccc1
phenol
[Al+3].[Br-].[Br-].[Br-]
aluminum tribromide
BrC12CC3CC(C1)CC(Br)(C3)C2
1,3-dibromoadamantane
Oc1ccc(C23CC4CC(C2)CC(c2ccc(O)cc2)(C4)C3)cc1
product
Oc1ccc(C23CC4CC(C2)CC(c2ccc(O)cc2)(C4)C3)cc1
1,3-bis(4-hydroxyphenyl)adamantane

Lösungsmittel

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeA 500 ml five-necked flask equipped with a thermometer, a stirrer, a reflux condenser, an inlet for nitrogen gas
  2. 2
    Sonstigea discharge pipe connected to a trap
  3. 3
    Temperaturwas cooled in an ice bath
  4. 4
    Waschenwashed with pure water
  5. 5
    workup.ADDITIONa saturated aqueous solution of sodium chloride and poured into methanol
  6. 6
    Sonstigeto separate the product
  7. 7
    SonstigeThe obtained product was dried under a reduced pressure

Vorschrift

A 500 ml five-necked flask equipped with a thermometer, a stirrer, a reflux condenser, an inlet for nitrogen gas and a discharge pipe connected to a trap containing a 30% by weight aqueous solution of sodium hydroxide was cooled in an ice bath. Into the flask, 6.47 g (0.022 moles) of 1,3-dibromoadamantane, 200 ml of phenol and 2.6 g (0.01 mole) of aluminum tribromide were placed. The resultant mixture was stirred at 0° C. for 6 hours and, then, the reaction was allowed to proceed under heating at 60° C. for 4 hours. The reaction product was poured into 2,000 liters of acidic ice water. After the ice melted, an organic layer was taken out, washed with pure water and a saturated aqueous solution of sodium chloride and poured into methanol to separate the product. The obtained product was dried under a reduced pressure, and 3.5 g of a product was obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08337982B2uspto-grants-2012_12