Hydrochloric Acid → 2,5-Bis-(10-hydroxydecoxy)terephthalic acid

HRID 378500Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 378500
[OH-].[K+].C([O:5][C:6](=[O:48])[C:7]1[CH:17]=[C:16]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][O:29]C(=O)C)[C:10]([C:11]([O:13]CC)=[O:12])=[CH:9][C:8]=1[O:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][O:44]C(=O)C)C.Cl>O.C(O)C>[OH:44][CH2:43][CH2:42][CH2:41][CH2:40][CH2:39][CH2:38][CH2:37][CH2:36][CH2:35][CH2:34][O:33][C:8]1[CH:9]=[C:10]([C:11]([OH:13])=[O:12])[C:16]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][OH:29])=[CH:17][C:7]=1[C:6]([OH:48])=[O:5]

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 19354086Diethyl-2,5-bis-(10-acetoxydecoxy)terephthalate

Produkt 1

HCID 193540842,5-Bis-(10-hydroxydecoxy)terephthalic acid

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of 20.0 g (303 mmol) 85% aqueous KOH in 200 ml water is added to 38.0 g (58.4 mmol) diethyl-2,5-bis-(10-acetoxydecoxy)terephthalate in 200 ml ethanol and the whole is heated under reflux for 1.5 hours. 28.0 ml conc. HCl are then added dropwise with ice-cooling and stirring until the solution shows an acidic pH. The precipitated, colourless crude product is filtered off, washed neutral and recrystallized from ethanol and methanol/acetone.

Aufarbeitung

  1. temperaturethe whole is heated
  2. temperatureunder reflux for 1.5 hours
  3. temperaturecooling
  4. filtrationThe precipitated, colourless crude product is filtered off
  5. washwashed neutral
  6. customrecrystallized from ethanol and methanol/acetone

Quellen und Nachweise

ORD-Eintrag
ord-0261dc4412834aa6b2f1b69ea546e9a6
Quelldatensatz
uspto-grants-2000_02
Patentnummer
US06031015

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