Triethylamine → p-Ethoxalyloxyethylstyrene

HRID 6407

Reaktionsgleichung

Reaktionsgleichung von HRID 6407
[OH:1][CH2:2][CH2:3][C:4]1[CH:11]=[CH:10][C:7]([CH:8]=[CH2:9])=[CH:6][CH:5]=1.C(N(CC)CC)C.[C:19](Cl)([C:21]([O:23][CH2:24][CH3:25])=[O:22])=[O:20]>C1C=CC=CC=1>[C:19]([O:1][CH2:2][CH2:3][C:4]1[CH:11]=[CH:10][C:7]([CH:8]=[CH2:9])=[CH:6][CH:5]=1)([C:21]([O:23][CH2:24][CH3:25])=[O:22])=[O:20]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 20884Ethoxalyl chlorideHCID 220518322-(4-Vinylphenyl)ethanol

Produkt 1

HCID 67847970p-Ethoxalyloxyethylstyrene

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Reaktionsbedingungen

Temperatur
10 °C

Versuchsvorschrift

A 200 ml flask equipped with a stirrer, a thermometer and a dropping funnel was charged with 14.8 g (0.1 mol) of p-hydroxyethylstyrene, 150 ml of benzene and 10.1 g (0.1 mol) of triethylamine and cooled to 10° C. To the mixture was added dropwise with stirring 13.7 g (0.1 mol) of ethoxalyl chloride for one hour at 10° C. to precipitate a hydrochloride of triethylamine (white solid). After mixting at room temperature for 2 hours, 80 g of hexane was added to complete precipitation of the hydrochloride. The hydrochloride is removed by filteration and the resultant filtrate was condensed to obtain the aimed compound. The compound was identified by 1H NMR (360 Mz) and IR. ##STR7##

Aufarbeitung

  1. customA 200 ml flask equipped with a stirrer
  2. additionTo the mixture was added dropwise
  3. customto precipitate a hydrochloride of triethylamine (white solid)
  4. addition80 g of hexane was added to complete precipitation of the hydrochloride
  5. customThe hydrochloride is removed by filteration
  6. customcondensed

Quellen und Nachweise

ORD-Eintrag
ord-eb42087260a94c678501a68bb3d83b03
Quelldatensatz
uspto-grants-1993_09
Patentnummer
US05248749

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