Ethylene Glycol → HCID 54458722, Verbindung

HRID 1438918

Reaktionsgleichung

Reaktionsgleichung von HRID 1438918
[CH3:1][O:2][C:3](=[O:14])[CH2:4][CH2:5][C:6]1([CH3:13])[CH2:11][CH2:10][CH2:9][CH2:8][C:7]1=O.[CH2:15]([OH:18])[CH2:16]O.[C:19]1([CH3:29])C=CC(S(O)(=O)=O)=CC=1.[OH2:30]>C1C=CC=CC=1>[CH3:1][O:2][C:3](=[O:14])[CH2:4][CH2:5][C:6]1([CH3:13])[CH2:11][CH2:10][CH2:9][CH2:8][C:7]21[C:15](=[O:18])[CH2:16][CH2:29][C:19]2=[O:30]

Komponenten

6

Edukt 4

HCID 174Ethylene GlycolHCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 574325Methyl 3-(1-methyl-2-oxocyclohexyl)propanoate

Produkt 1

HCID 54458722HCID 54458722, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel2×

Versuchsvorschrift

A solution of 1-methyl-2-oxocyclohexanepropionic acid methyl ester (96.1 g, 0.48 mole), described in Example 6, ethylene glycol (100 ml) and p-toluenesulfonic acid (2.0 g) in dry benzene (1600 ml) is heated at reflux for 6 hr using a water separator. The benzene solution is cooled, washed with saturated aqueous sodium bicarbonate solution (2 × 100 ml) then brine (2 × 100 ml), dried (MgSO4) and concentrated to yield the title compound as an oil, ν maxCHCl3 1725, 1085 cm-1.

Aufarbeitung

  1. temperatureis heated
  2. temperatureat reflux for 6 hr
  3. washwashed with saturated aqueous sodium bicarbonate solution (2 × 100 ml)
  4. dry with materialbrine (2 × 100 ml), dried (MgSO4)
  5. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-c73c0e10c4f24e459151ea5a2f68d76c
Quelldatensatz
uspto-grants-1977_11
Patentnummer
US04057559

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