Ethylene Glycol → HCID 59253950, Verbindung

HRID 501853Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 501853
Cl.[N+:2]([C:5]1[CH:19]=[CH:18][C:8]([O:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][C:15]([OH:17])=[O:16])=[CH:7][CH:6]=1)([O-:4])=[O:3].[CH2:20](O)[CH2:21][OH:22]>>[OH:22][CH2:21][CH2:20][O:16][C:15](=[O:17])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][O:9][C:8]1[CH:7]=[CH:6][C:5]([N+:2]([O-:4])=[O:3])=[CH:19][CH:18]=1

Komponenten

4

Edukt 3

HCID 174Ethylene GlycolHCID 313Hydrochloric Acid2×HCID 223889056-(4-Nitrophenoxy)hexanoic acid

Produkt 1

HCID 59253950HCID 59253950, Verbindung

Versuchsvorschrift

Dry HCl gas was passed through a mixture of 6-(4-nitrophenoxy)-hexanoic acid 35 (50 g, 197.62 mmol) and ethylene glycol (200 ml) was passed dry HCl gas for one hour. During HCl gas bubbling the temperature rose to 60° C. The crude reaction mass was poured onto ice (1 kg), extracted in to ethyl acetate, washed with water (2×250 ml), dried over sodium sulphate and distilled to get crude 36, which was purified by column chromatography on silica gel using benzene as eluant to get pure 36 (46 g, 78.3) as a light yellow syrup.

Aufarbeitung

  1. customfor one hour
  2. customDuring HCl gas bubbling the temperature
  3. customrose to 60° C
  4. customThe crude reaction mass
  5. additionwas poured onto ice (1 kg)
  6. extractionextracted in to ethyl acetate
  7. washwashed with water (2×250 ml)
  8. dry with materialdried over sodium sulphate
  9. distillationdistilled
  10. customto get crude 36, which
  11. customwas purified by column chromatography on silica gel
  12. customto get pure 36 (46 g, 78.3) as a light yellow syrup

Quellen und Nachweise

ORD-Eintrag
ord-19bd02dd0c4a4823b2f4c8a67b219065
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07772352B2

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