Selenium Dioxide → 2-Methoxyphenylglyoxal hydrate

HRID 66318

Reaktionsgleichung

Reaktionsgleichung von HRID 66318
C[O:2][CH2:3][C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:5].[Se](=O)=O.[O:15]1CCOC[CH2:16]1>O.C(OCC)(=O)C>[OH2:2].[CH3:16][O:15][C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=1[C:4]([CH:3]=[O:2])=[O:5]

Komponenten

6

Edukt 3

HCID 24007Selenium DioxideHCID 312751,4-DioxaneHCID 776982-Methoxy-1-phenylethanone

Produkt 1

HCID 204341102-Methoxyphenylglyoxal hydrate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

3 g of 2-methoxyacetophenone are dissolved in 15 ml of dioxane, and a solution of 3.3 g of selenium dioxide in 1.5 ml of water is added thereto. The solution is refluxed for 15 hours. After the reaction, insoluble materials are removed by filtration, and the filtrate is concentrated. The oily residue thus obtained is dissolved in ethyl acetate. The ethyl acetate solution is washed with water and then with an aqueous sodium bicarbonate solution and water. Then, said solution is dried and evaporated to remove solvent. 3.1 g of 2-methoxyphenylglyoxal hydrate are obtained as a crude oil.

Aufarbeitung

  1. temperatureThe solution is refluxed for 15 hours
  2. customAfter the reaction, insoluble materials
  3. customare removed by filtration
  4. concentrationthe filtrate is concentrated
  5. customThe oily residue thus obtained
  6. washThe ethyl acetate solution is washed with water
  7. customis dried
  8. customevaporated
  9. customto remove solvent

Quellen und Nachweise

ORD-Eintrag
ord-d7ae0d83b4204e4da29186e8c627e9d9
Quelldatensatz
uspto-grants-1978_12
Patentnummer
US04131686

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