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Sodium Hydroxide → 5-Methyl-4,5-dihydro-4-oxo-pyrrolo[1,2-a]quinoxaline-2-carboxylic acid

HRID 26703
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반응식

HRID 26703 반응식
[OH-].[Na+].[CH3:3][N:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[N:7]2[CH:14]=[C:15]([C:17]([O:19]CC)=[O:18])[CH:16]=[C:6]2[C:5]1=[O:22]>O.C(O)C>[CH3:3][N:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[N:7]2[CH:14]=[C:15]([C:17]([OH:19])=[O:18])[CH:16]=[C:6]2[C:5]1=[O:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 14067565Ethyl 5-methyl-4,5-dihydro-4-oxo-pyrrolo[1,2-a]quinoxaline-2-carboxylate

생성물 1

HCID 140675775-Methyl-4,5-dihydro-4-oxo-pyrrolo[1,2-a]quinoxaline-2-carboxylic acid수율 95%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A solution of 0.9 g of sodium hydroxide in 50 ml of water was added to a suspension of 1.66 g of ethyl 5-methyl-4,5-dihydro-4-oxo-pyrrolo[1,2-a]quinoxaline-2-carboxylate in 30 ml of hot ethanol and the mixture was warmed on a water bath for one hour after which thin layer chromatography showed no ester present. The resulting solution was filtered hot and the filtrate was acidified to a pH of 1-2 with concentrated hydrochloric acid. The mixture was cooled and filtered and the recovered product was rinsed with water and dried over P2O5 under vacuum to obtain 1.40 g (95% yield) of 5-methyl-4,5-dihydro-4-oxo-pyrrolo[1,2-a]quinoxaline-2-carboxylic acid melting at 330°-333° C.

후처리

  1. temperaturethe mixture was warmed on a water bath for one hour after which thin layer chromatography
  2. filtrationThe resulting solution was filtered hot
  3. temperatureThe mixture was cooled
  4. filtrationfiltered
  5. washthe recovered product was rinsed with water
  6. dry with materialdried over P2O5 under vacuum

출처 및 근거

ORD 기록
ord-5c9f561fc25d4670834c2e2a4de290cd
출처 데이터셋
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04151280

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