Potassium Iodide → 1,1'-Oxybis(2,2-diethoxyethane)

HRID 1596329

Reaktionsgleichung

Reaktionsgleichung von HRID 1596329
[CH2:1]([O:3][CH:4]([O:7][CH2:8][CH3:9])[CH2:5][OH:6])[CH3:2].[H-].[Na+].[CH2:12]([O:14][CH:15]([O:18][CH2:19][CH3:20])[CH2:16]Br)[CH3:13].[I-].[K+]>O1CCCC1.O>[CH2:1]([O:3][CH:4]([O:7][CH2:8][CH3:9])[CH2:5][O:6][CH2:16][CH:15]([O:18][CH2:19][CH3:20])[O:14][CH2:12][CH3:13])[CH3:2]

Komponenten

7

Edukt 4

HCID 4875Potassium IodideHCID 121292,2-DiethoxyethanolHCID 24758Sodium hydrideHCID 74852Ethane, 2-bromo-1,1-diethoxy-

Produkt 1

HCID 926201,1'-Oxybis(2,2-diethoxyethane)

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Hydroxyacetaldehyde diethylacetal (3.75 g) was added to sodium hydride (0.8 g, 80% in mineral oil) in tetrahydrofuran (100 ml) under an atmosphere of nitrogen. The mixture was stirred and bromoacetaldehyde diethyl acetal (5.0 g) and potassium iodide (0.1 g) were added. The mixture was heated to reflux for 16 hours, water added and evaporated under reduced pressure. The residue was dissolved in diethyl ether, the organic phase washed with water, dried (MgSO4) and evaporated under reduced pressure to give bis(2,2-diethoxyethyl)ether, 3.43 g, as a yellow oil.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 16 hours
  3. customevaporated under reduced pressure
  4. dissolutionThe residue was dissolved in diethyl ether
  5. washthe organic phase washed with water
  6. dry with materialdried (MgSO4)
  7. customevaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-762dd13dd60b46679156dd68420a4155
Quelldatensatz
uspto-grants-2001_09
Patentnummer
US06291474B1

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