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

HRID 1658050

反応式

HRID 1658050 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 the supernatant 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-afc1d461701f476293a357a7224491fa
出典データセット
uspto-grants-1976_06
特許番号
US03962440

関連ノート

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