Ethylene Glycol → 2-(3-Bromo-o-tolyl)-2-methyl-1,3-dioxolane

HRID 1439562Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1439562
[Br:1][C:2]1[C:3](C)=[C:4]([C:8](=O)C)[CH:5]=[CH:6][CH:7]=1.[C:12]1(C)C=CC(S(O)(=O)=O)=C[CH:13]=1.[C:23](=[O:26])([O-])[O-:24].[Na+].[Na+].[CH2:29](O)CO>O.C1(C)C=CC=CC=1>[Br:1][C:2]1[C:3]([C:23]2([CH3:29])[O:26][CH2:13][CH2:12][O:24]2)=[C:4]([CH3:8])[CH:5]=[CH:6][CH:7]=1

Komponenten

7

Edukt 4

HCID 174Ethylene Glycol2×HCID 6101p-Toluenesulfonic acidHCID 10340Sodium CarbonateHCID 204801311-(3-Bromo-2-methylphenyl)ethanone

Produkt 1

HCID 706381482-(3-Bromo-o-tolyl)-2-methyl-1,3-dioxolane

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 1140TolueneLösungsmittel

Versuchsvorschrift

A mixture of 100 parts of 3'-bromo-2'-methylacetophenone, 30 parts of ethylene glycol, 320 parts of anhydrous toluene and 2 parts of p-toluenesulfonic acid is stirred and refluxed for 4 hours with water-separator. A second fraction of 30 parts of ethylene glycol is added and stirring at reflux is continued for 18 hours. The reaction mixture is cooled and stirred for 30 minutes with 5 parts of sodium carbonate. The organic layer is separated, washed twice with water, dried and evaporated. The residue is distilled twice, yielding 2-(3-bromo-o-tolyl)-2-methyl-1,3-dioxolane; bp. 148°-150° C at 12 mm. pressure.

Aufarbeitung

  1. stirringstirring
  2. temperatureat reflux
  3. temperatureThe reaction mixture is cooled
  4. customThe organic layer is separated
  5. washwashed twice with water
  6. customdried
  7. customevaporated
  8. distillationThe residue is distilled twice

Quellen und Nachweise

ORD-Eintrag
ord-163c695b0c3a46ebbc4f0d93b07454dd
Quelldatensatz
uspto-grants-1977_11
Patentnummer
US04060528

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