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HCID 19990445, 화합물 → 1-Hydroxy-6-(trifluoromethyl)-1,4-dihydroquinoxaline-2,3-dione

HRID 346151
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HRID 346151 반응식
[C:1]([NH:8][C:9]1[CH:10]=[C:11]([C:18]([F:21])([F:20])[F:19])[CH:12]=[CH:13][C:14]=1[N+:15]([O-])=[O:16])([C:3](OCC)=[O:4])=[O:2]>C(O)C.[Pt]>[OH:16][N:15]1[C:14]2[C:9](=[CH:10][C:11]([C:18]([F:21])([F:20])[F:19])=[CH:12][CH:13]=2)[NH:8][C:1](=[O:2])[C:3]1=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 19990445HCID 19990445, 화합물

생성물 1

HCID 199904361-Hydroxy-6-(trifluoromethyl)-1,4-dihydroquinoxaline-2,3-dione수율 36.6%

시약·촉매·용매 2

HCID 23939Platinum촉매HCID 702Ethanol용매

실험 절차

A solution of 3-ethoxalylamino-4-nitrobenzotrifluoride (0.61 g, 2 mmol) in 50 ml of 96% ethanol was hydrogenated at atmospheric pressure and room temperature in the presence of 30 mg of 5% platinum on carbon for 5 min. The catalyst was filtered off and washed with ethanol. Acetic acid (10 ml) was added to the filtrate and the solution was refluxed for 1.5 h. The mixture was evaporated to dryness, and the residue was recrystallized from ethanol/water to give 0.18 g (36%) of the title compound. M.p.>220° C. dec.; 1H-NMR (DMSO-d6): 7.40-7.70 (m, 3H, ArH), 12.1 (broad s, 1H, NH); IR (KBr): 1700, 1625 cm-1 ; MS (m/e): 246 (68%, M+).

후처리

  1. filtrationThe catalyst was filtered off
  2. washwashed with ethanol
  3. additionAcetic acid (10 ml) was added to the filtrate
  4. temperaturethe solution was refluxed for 1.5 h
  5. customThe mixture was evaporated to dryness
  6. customthe residue was recrystallized from ethanol/water

출처 및 근거

ORD 기록
ord-0625376e29e642d8aa2aba16dbf870e9
출처 데이터셋
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05061706

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