Hydrogen Peroxide → 1-Methyl-1,4-dihydro-2,3-quinoxalinedione

HRID 1730269

Reaktionsgleichung

Reaktionsgleichung von HRID 1730269
[CH3:1][N:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[CH:4][C:3]1=[O:12].[OH:13]O>C(O)(=O)C>[CH3:1][N:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[NH:5][C:4](=[O:13])[C:3]1=[O:12]

Komponenten

4

Edukt 2

HCID 784Hydrogen PeroxideHCID 3514291-Methyl-1,2-dihydroquinoxalin-2-one

Produkt 1

HCID 6006271-Methyl-1,4-dihydro-2,3-quinoxalinedione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

1-Methyl-2(1H)-quinoxalinone (5.3 grams) was allowed to stand at room temperature for 72 hours in a mixture of 60 ml. of acetic acid and 35 ml. of 30 percent hydrogen peroxide. The product separated out as needles after 48 hours. After 72 hours, no starting material was detectable in thesupernatant liquid by TLC (ethyl acetate). The product was separated and washed sequentially with water and with ethanol, m.p. 287°-289° C. It was then recrystallized from water, 287°-290° C. (literature: 286°-287° C., G. W. H. Cheeseman, J. Chem. Soc. 1804 (1955); 285°-286° C., G. W.H. Cheeseman, J. Chem. Soc. 1246 (1961)). NMR also confirmed the identity of the product.

Aufarbeitung

  1. additionto stand at room temperature for 72 hours in a mixture of 60 ml
  2. customThe product separated out as needles after 48 hours
  3. customThe product was separated
  4. washwashed sequentially with water and with ethanol, m.p. 287°-289° C
  5. customIt was then recrystallized from water, 287°-290° C. (literature: 286°-287° C., G. W. H. Cheeseman, J. Chem. Soc. 1804 (1955); 285°-286° C., G. W.H. Cheeseman, J. Chem. Soc. 1246 (1961))

Quellen und Nachweise

ORD-Eintrag
ord-30a8caf2dc5842e7bad6efc86bf393d0
Quelldatensatz
uspto-grants-1976_11
Patentnummer
US03992378

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