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

HRID 1730269

반응식

HRID 1730269 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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))

출처 및 근거

ORD 기록
ord-30a8caf2dc5842e7bad6efc86bf393d0
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03992378

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