Reacción #885

ord-bfcf42b524d14d69860f018538be3094

Ecuación de reacción

Oc1ccc(C2(c3ccc(O)cc3)c3ccccc3-c3ccccc32)cc1
9,9-bis(4-hydroxyphenyl)fluorene
O=C1OCCO1
ethylene carbonate
O=C([O-])[O-].[K+].[K+]
potassium carbonate
C1COCCOCCOCCOCCOCCO1
18-crown-6
OCCOc1ccccc1-c1cccc2c1-c1ccccc1C2
white powder
OCCOc1ccccc1-c1cccc2c1-c1ccccc1C2
4-(2-hydroxyethoxyphenyl)fluorene

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturaat reflux
  2. 2
    Otrothe solvent was decanted from the precipitated product
  3. 3
    LavadoThe resulting white solid was washed with ligroin (
  4. 4
    Otrodried under a stream of nitrogen
  5. 5
    OtroThe product was recrystallized from methanol

Procedimiento

A mixture of 84.4 g (0.241 mol) of 9,9-bis(4-hydroxyphenyl)fluorene, 46.7 g (0.53 mol) of ethylene carbonate, 3.3 g (0.024 mol) of potassium carbonate, and a catalytic amount of 18-crown-6 in 400 mL of xylenes was heated at reflux with mechanical stirring for 6 h. The mixture was allowed to cool slowly to room temperature, and the solvent was decanted from the precipitated product. The resulting white solid was washed with ligroin (to prevent the formation of a gummy mass), and dried under a stream of nitrogen. The product was recrystallized from methanol, providing 70.4 g (67%) of a white powder.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05723264uspto-grants-1998_03