Reaktion #2180447

ord-e4637182e36247888c7b686d71c1495b

Lösungsmittel

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISTILLATIONby distilling 5 mL of the solution
  2. 2
    TemperaturThe mixed solution was refluxed for 1 hour
  3. 3
    Sonstigewas 100° C.
  4. 4
    workup.DISTILLATIONhigher, distilled until the amount of the solution
  5. 5
    workup.DISTILLATIONAfter the distillation, volatile components of the residual mixed solution
  6. 6
    Sonstigewere vaporized under reduced pressure by a rotary evaporator
  7. 7
    Sonstigewere completely removed
  8. 8
    workup.DISSOLUTION1.89 g of catechol-aluminum complex was dissolved into 100 mL of 1:4 acetylacetone/toluene
  9. 9
    Sonstigeto produce a coating liquid

Vorschrift

A solution of catechol (3.30 g, 30.0 mmol) and toluene (45 ml) was dehydrated by distilling 5 mL of the solution. Thereafter, 4.08 g (20.0 mmol) of aluminum(III) isopropoxide was added to the solution while stirring. The mixed solution was refluxed for 1 hour, and then, while the distillation temperature was 100° C. or higher, distilled until the amount of the solution became half. After the distillation, volatile components of the residual mixed solution were vaporized under reduced pressure by a rotary evaporator. The residual solid content was further heated to 100° C. under vacuum using a vacuum dryer so that the remaining volatile components were completely removed. The solid content (catechol-aluminum complex) was green in color. The yield amount was 3.78 g (20.0 mmol), and the yield percentage was 100%. 1.89 g of catechol-aluminum complex was dissolved into 100 mL of 1:4 acetylacetone/toluene to produce a coating liquid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08445118B2uspto-grants-2013_05