Ethylene Glycol → 2-(2,6-Dimethyl-3-nitrophenyl)-1,3-dioxolane

HRID 619685

Reaktionsgleichung

Reaktionsgleichung von HRID 619685
[CH3:1][C:2]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[C:6]([CH3:13])[C:3]=1[CH:4]=[O:5].[CH2:14](O)[CH2:15][OH:16].C1(C)C=CC(S(O)(=O)=O)=CC=1.O>C1(C)C=CC=CC=1>[CH3:1][C:2]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[C:6]([CH3:13])[C:3]=1[CH:4]1[O:16][CH2:15][CH2:14][O:5]1

Komponenten

6

Edukt 4

HCID 174Ethylene GlycolHCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 218470162,6-Dimethyl-3-nitrobenzaldehyde

Produkt 1

HCID 218470332-(2,6-Dimethyl-3-nitrophenyl)-1,3-dioxolane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

A solution of 2.8 g of 2,6-dimethyl-3-nitrobenzaldehyde in 150 ml of toluene was treated with 5 ml of ethylene glycol and 20 mg of p-toluenesulphonic acid. The mixture was heated to reflux for 18 hours, with the water being separated using a separator. The mixture was left to cool to room temperature and was washed twice with water. After drying over anhydrous magnesium sulphate the solvent was evaporated and the crystalline residue was crystallized from hexane. 3.0 g of 2-(2,6-dimethyl-3-nitrophenyl)-1,3-dioxolane, m.p. 69-71° C., were obtained.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. customseparated
  3. waitThe mixture was left
  4. washwas washed twice with water
  5. dry with materialAfter drying over anhydrous magnesium sulphate the solvent
  6. customwas evaporated
  7. customthe crystalline residue was crystallized from hexane

Quellen und Nachweise

ORD-Eintrag
ord-665e51ad9b7543fe8ead1b6b9ca316c0
Quelldatensatz
uspto-grants-1999_09
Patentnummer
US05959113

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