1-Octanol → Tetraoctyl pyromellitate

HRID 2068473Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2068473
[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].[CH2:19](O)[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26]>CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-].[Ti+4].C1(C)C(C)=CC=CC=1>[CH2:19]([O:14][C:13](=[O:15])[C:12]1[C:8](=[CH:7][C:3](=[C:2]([CH:16]=1)[C:1]([O:18][CH2:9][CH2:8][CH2:7][CH2:3][CH2:2][CH2:16][CH2:12][CH3:13])=[O:17])[C:4]([O:6][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])=[O:5])[C:9]([O:11][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])=[O:10])[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26]

Komponenten

5

Edukt 2

HCID 9571-OctanolHCID 6961Pyromellitic Acid

Produkt 1

HCID 21895707Tetraoctyl pyromellitateAusbeute 209 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 11026Titanium isopropoxideKatalysatorHCID 7237O-XyleneLösungsmittel

Versuchsvorschrift

To a 2-liter four necked flask equipped with Dean Stark, 218 g of anhydrous pyromellitic acid, 650 g of n-octanol, 0.2 g of titanium tetraisopropoxide and 300 ml of xylene were added and reacted with agitation at 160 degrees C. for 4 hours under nitrogen stream while distilling water. Subsequently, washing by saturated saline and washing by 0.1 N aqueous sodium hydroxide were respectively conducted three times, followed by being dried by anhydrous magnesium sulfate. After magnesium sulfate was filtered, unreacted alcohol was distilled under diminished pressure to obtain 630 g of pyromellitic acid tetraoctyl ester as a residue. The obtained compound, regarded as Comparative 1-3, was similarly measured with respect to the properties.

Aufarbeitung

  1. additionwere added
  2. customreacted with agitation at 160 degrees C
  3. distillationfor 4 hours under nitrogen stream while distilling water
  4. washSubsequently, washing by saturated saline
  5. washwashing by 0.1 N aqueous sodium hydroxide
  6. dry with materialby being dried by anhydrous magnesium sulfate
  7. filtrationAfter magnesium sulfate was filtered
  8. distillationunreacted alcohol was distilled under diminished pressure

Quellen und Nachweise

ORD-Eintrag
ord-87aba8bd25644d599c437a05a7dc0ce2
Quelldatensatz
uspto-grants-2012_10
Patentnummer
US08299004B2

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