Reaktion #2208280

ord-82df646569fa474eb94813285ba91a8c

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeIn a 500 mL flask equipped with magnetic stirring bar
  2. 2
    Temperaturwas maintained
  3. 3
    SonstigeThen the reaction was quenched with water/NaHCO3
  4. 4
    Sonstigethe organic layer was separated
  5. 5
    Waschenwashed with water
  6. 6
    SonstigeThe crude product was crystallized
  7. 7
    Sonstigeupon standing at room temperature
  8. 8
    Sonstigewas further purified
  9. 9
    Waschenby washing with pentane or MeOH

Vorschrift

In a 500 mL flask equipped with magnetic stirring bar were introduced 4.46 g (0.023 moles) of 1-phenyl-indene, 0.35 g (0.0117 moles) of formalin and 0.88 g (0.0046 moles) of para-toluenesulphonic acid in 200 ml of toluene; the mixture was heated to 80° C. and was maintained under stirring for 6 hours at 80° C. Then the reaction was quenched with water/NaHCO3; the organic layer was separated, washed with water and brought to dryness under reduced pressure. The crude product was crystallized upon standing at room temperature, and then was further purified by washing with pentane or MeOH, thus isolating 4.5 g of bis(3-phenyl-2-indenyl)methane (purity of 97.3% by G.C.; yield=95.2%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06693156B1uspto-grants-2004_02