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Acetic Acid → 5-methoxy-3-methyl-1H-quinazoline-2,4-dione

HRID 598071
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HRID 598071 반응식
[CH3:1][O:2][C:3]1[CH:12]=[CH:11][CH:10]=[C:9]([NH:13][C:14]([NH:16][CH3:17])=[O:15])[C:4]=1[C:5](NC)=[O:6].[OH-].[Na+].C(O)(=O)C>O.C(O)C>[CH3:1][O:2][C:3]1[CH:12]=[CH:11][CH:10]=[C:9]2[C:4]=1[C:5](=[O:6])[N:16]([CH3:17])[C:14](=[O:15])[NH:13]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 176Acetic AcidHCID 14798Sodium HydroxideHCID 672680242-Methoxy-N-methyl-6-[[(methylamino)carbonyl]amino]benzamide

생성물 1

HCID 672670575-methoxy-3-methyl-1H-quinazoline-2,4-dione수율 97%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A mixture of 2-Methoxy-N-methyl-6-[[(methylamino)carbonyl]amino]benzamide (200 mg, 0.843 mmol), 5% sodium hydroxide solution in water (8 ml) and ethanol (4 ml) was refluxed for 1 h. The solution was allowed to cool and then acidified with acetic acid. The aqueous solution was extracted with ethyl acetate. The extract was washed with brine, dried over magnesium sulfate, and concentrated under vacuum to afford 168 mg (97%) of the title compound.

후처리

  1. temperaturewas refluxed for 1 h
  2. temperatureto cool
  3. extractionThe aqueous solution was extracted with ethyl acetate
  4. washThe extract was washed with brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-7be018ffceb44458a5f7a83ce0c4a6e1
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07897607B2

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