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

HRID 1730269

反応式

HRID 1730269 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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.

後処理

  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))

出典と根拠

ORDレコード
ord-30a8caf2dc5842e7bad6efc86bf393d0
出典データセット
uspto-grants-1976_11
特許番号
US03992378

関連ノート

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