Pyromellitic Acid → 1,2,4,5-Cyclohexanetetracarboxylic Acid

HRID 1518778

Reaktionsgleichung

Reaktionsgleichung von HRID 1518778
[C:1]([OH:18])(=[O:17])[C:2]1[C:3](=[CH:7][C:8](=[C:12]([CH:16]=1)[C:13]([OH:15])=[O:14])[C:9]([OH:11])=[O:10])[C:4]([OH:6])=[O:5].[H][H]>[Rh].O>[CH:8]1([C:9]([OH:11])=[O:10])[CH2:7][CH:3]([C:4]([OH:6])=[O:5])[CH:2]([C:1]([OH:18])=[O:17])[CH2:16][CH:12]1[C:13]([OH:15])=[O:14]

Komponenten

5

Edukt 2

HCID 6961Pyromellitic AcidHCID 178418361HCID 178418361, Verbindung4×

Produkt 1

HCID 28349461,2,4,5-Cyclohexanetetracarboxylic AcidAusbeute 85,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23948RhodiumKatalysatorHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

A 5 L-capacity Hastelloy (HC22) autoclave was charged with 552 g of pyromellitic acid, 200 g of a catalyst prepared by supporting rhodium on activated carbon (available from N.E. Chemcat Corp.) and 1656 g of water, and while stirring the contents of the autoclave, an interior of the reaction vessel was replaced with a nitrogen gas. Then, the interior of the reaction vessel was replaced with a hydrogen gas until a hydrogen pressure in the reaction vessel reached 5.0 MPa and an inside temperature of the reaction vessel was raised up to 60° C. The contents of the autoclave were reacted for 2 hours while maintaining a hydrogen pressure in the autoclave at 5.0 MPa. The hydrogen gas in the reaction vessel was replaced with a nitrogen gas, and the obtained reaction solution was withdrawn from the autoclave. The thus obtained reaction solution was subjected to hot filtration to separate the catalyst therefrom. The resulting filtrate was concentrated by evaporating water therefrom under reduced pressure using a rotary evaporator to precipitate crystals, and the resulting slurry was subjected to solid-liquid separation at room temperature to separate the precipitated crystals therefrom. The thus obtained crystals were dried to obtain 481 g of 1,2,4,5-cyclohexane tetracarboxylic acid (yield: 85.0%).

Aufarbeitung

  1. customprepared
  2. customThe contents of the autoclave were reacted for 2 hours
  3. customthe obtained reaction solution
  4. customwas withdrawn from the autoclave
  5. customThe thus obtained reaction solution
  6. filtrationwas subjected to hot filtration
  7. customto separate the catalyst
  8. concentrationThe resulting filtrate was concentrated
  9. customby evaporating water
  10. customa rotary evaporator
  11. customto precipitate crystals
  12. customthe resulting slurry was subjected to solid-liquid separation at room temperature
  13. customto separate the precipitated crystals
  14. customThe thus obtained crystals were dried

Quellen und Nachweise

ORD-Eintrag
ord-0e310f3c408843ed926a70708550c891
Quelldatensatz
uspto-grants-2015_07
Patentnummer
US09073297B2

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