Methylparaben → HCID 54331531, Verbindung

HRID 1788770Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1788770
[CH3:1][O:2][C:3](=[O:11])[C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1.[CH2:12]([CH:14]([CH2:17][CH2:18][CH2:19][CH3:20])[CH2:15]Cl)[CH3:13].C[O-].[Na+]>CN(C)C=O>[CH3:1][O:2][C:3](=[O:11])[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH2:15][CH:14]([CH2:12][CH3:13])[CH2:17][CH2:18][CH2:19][CH3:20])=[CH:6][CH:5]=1

Komponenten

5

Edukt 3

HCID 7456MethylparabenHCID 312402-Ethylhexyl chlorideHCID 10942334Sodium Methoxide

Produkt 1

HCID 54331531HCID 54331531, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture of 51.7 g (0.34 mol) of 4-hydroxybenzoic acid methylester, 500 ml of dimethyl formamide, 60 g (0.40 mol) of 2-ethylhexylchloride and 21.8 g (0.40 mol) of sodium methylate was heated for 7 hours to boiling temperature and, after cooling and removal of the sodium chloride by filtration, was evaporated to dryness under reduced pressure. The residue was dissolved in methylene chloride and chromatographed (eluent: methylene chloride) on silica gel (Merck) to yield 43 g (48% of the theoretical) of 4-(2-ethylhexyloxy)benzoic acid methylester. A refractive index of

Aufarbeitung

  1. temperaturewas heated for 7 hours
  2. temperatureafter cooling
  3. customremoval of the sodium chloride
  4. filtrationby filtration
  5. customwas evaporated to dryness under reduced pressure
  6. dissolutionThe residue was dissolved in methylene chloride
  7. customchromatographed (eluent: methylene chloride) on silica gel (Merck)

Quellen und Nachweise

ORD-Eintrag
ord-145a27aebfd74767a69e19e03a8c59f6
Quelldatensatz
uspto-grants-1987_08
Patentnummer
US04684665

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