Sodium Iodide → Diethyl-2,5-bis-(10-bromodecoxy)terephthalate

HRID 378498

Reaktionsgleichung

Reaktionsgleichung von HRID 378498
[CH2:1]([O:3][C:4](=[O:18])[C:5]1[CH:15]=[C:14]([OH:16])[C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:7][C:6]=1[OH:17])[CH3:2].Br[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][Br:30].C([O-])([O-])=O.[K+].[K+].[Na+].[I-]>CC(C)=O>[CH2:1]([O:3][C:4](=[O:18])[C:5]1[CH:15]=[C:14]([O:16][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][Br:30])[C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:7][C:6]=1[O:17][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][Br:30])[CH3:2]

Komponenten

6

Edukt 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 79980Diethyl 2,5-dihydroxyterephthalateHCID 2214831,10-Dibromodecane

Produkt 1

HCID 19354090Diethyl-2,5-bis-(10-bromodecoxy)terephthalate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

25.4 g (0.1 mol) diethyl-2,5-dihydroxyterephthalate, 450 g (1.5 mol) 1,10-dibromodecane, 138 g (1.0 mol) K2CO3 and 200 mg NaI in 200 ml acetone are heated under reflux for 28 hours until the originally yellow suspension has decolorized. After distilling off the solvent, the reaction mixture is extracted twice with diethyl ether (2×250 ml), and insoluble salts are filtered off. The filtrate is washed twice with 200 ml water and dried over Na2SO4. The solvent is then distilled off. The colourless, solid residue is washed twice with petroleum ether and then recrystallized from petroleum ether.

Aufarbeitung

  1. temperatureunder reflux for 28 hours until the originally yellow suspension
  2. distillationAfter distilling off the solvent
  3. extractionthe reaction mixture is extracted twice with diethyl ether (2×250 ml), and insoluble salts
  4. filtrationare filtered off
  5. washThe filtrate is washed twice with 200 ml water
  6. dry with materialdried over Na2SO4
  7. distillationThe solvent is then distilled off
  8. washThe colourless, solid residue is washed twice with petroleum ether
  9. customrecrystallized from petroleum ether

Quellen und Nachweise

ORD-Eintrag
ord-8771b1594f4a446fb4425ec5b0c79c75
Quelldatensatz
uspto-grants-2000_02
Patentnummer
US06031015

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