Ethylene Glycol → HCID 56626634, Verbindung

HRID 66466

Reaktionsgleichung

Reaktionsgleichung von HRID 66466
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH:12]([N+:25]([O-:27])=[O:26])[CH2:13][CH2:14][C:15](=[O:24])[CH2:16][CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].C1(C)C=CC(S(O)(=O)=O)=CC=1.[CH2:39](O)[CH2:40][OH:41]>C1CCCCC1>[CH2:40]1[O:41][C:15]([CH2:16][CH2:17][C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)([CH2:14][CH2:13][CH:12]([N+:25]([O-:27])=[O:26])[CH2:11][C:5]2[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=2)[O:24][CH2:39]1

Komponenten

5

Edukt 3

HCID 174Ethylene GlycolHCID 6101p-Toluenesulfonic acidHCID 201642191-(3',4'-Dimethoxyphenyl)-7-phenyl-2-nitro-5-heptanone

Produkt 1

HCID 56626634HCID 56626634, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8078CyclohexaneLösungsmittel

Versuchsvorschrift

Into a 1 l r.b. flask equipped with a Dean Stark trap was placed 46.4 g (0.12 m) of 1-(3',4'-dimethoxyphenyl)-7-phenyl-2-nitro-5-heptanone, 1.5 g p-toluenesulfonic acid, 50 mL of ethylene glycol and 300 mL of cyclohexane. The mixture was allowed to reflux overnight, then concentrated in vacuo. Dil NaHCO3 solution was added to the residue and extracted with ethyl acetate. The organic layer was backwashed with water, dried over anh. MgSO4, filtered and concentrated under reduced pressure to give 45.3 g of an oil which solidified on drying at room temperature under vacuum.

Aufarbeitung

  1. customflask equipped with a Dean Stark trap
  2. temperatureto reflux overnight
  3. concentrationconcentrated in vacuo
  4. additionDil NaHCO3 solution was added to the residue
  5. extractionextracted with ethyl acetate
  6. dry with materialdried over anh. MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-cff983f688d644729605de86f7b460a4
Quelldatensatz
uspto-grants-1982_08
Patentnummer
US04342692

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