HCID 86628083, 화합물 → HCID 67037355, 화합물

HRID 1401299노트

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HRID 1401299 반응식
[C:1](/[C:5]1[C:6]([C:12]([F:15])([F:14])[F:13])=[N+:7]([O-:11])[CH:8]=[CH:9][CH:10]=1)(=[N:3]\[NH2:4])\[NH2:2].[CH3:16][O:17][C:18]1[CH:19]=[C:20]([C:29](=O)[CH:30]=O)[CH:21]=[C:22]([N+:26]([O-:28])=[O:27])[C:23]=1[O:24][CH3:25]>C(O)C>[CH3:16][O:17][C:18]1[CH:19]=[C:20]([C:29]2[N:2]=[C:1]([C:5]3[C:6]([C:12]([F:13])([F:15])[F:14])=[N+:7]([O-:11])[CH:8]=[CH:9][CH:10]=3)[N:3]=[N:4][CH:30]=2)[CH:21]=[C:22]([N+:26]([O-:28])=[O:27])[C:23]=1[O:24][CH3:25]

참가 물질

4

반응물 2

HCID 86628083HCID 86628083, 화합물HCID 87244702HCID 87244702, 화합물

생성물 1

HCID 67037355HCID 67037355, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a stirred solution of (Z)-3-carbamohydrazonoyl-2-(trifluoromethyl)pyridine 1-oxide (1.10 g, 5 mmol) in ethanol (30 mL) was added 2-(3,4-dimethoxy-5-nitrophenyl)-2-oxoacetaldehyde (1.19 g, 5 mmol). The reaction mixture was heated to reflux for 5 hours, and then cooled to room temperature and the solvent was removed by evaporation. The residue was dissolved in dichloromethane (30 mL) and the organic phase was washed with water and dried over anhydrous magnesium sulphate, filtered and evaporated. The crude product was recrystallized from isopropanol to give 3-(5-(3,4-dimethoxy-5-nitrophenyl)-1,2,4-triazin-3-yl)-2-(trifluoromethyl)pyridine 1-oxide, 1.69 g (80%).

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 5 hours
  3. customthe solvent was removed by evaporation
  4. dissolutionThe residue was dissolved in dichloromethane (30 mL)
  5. washthe organic phase was washed with water
  6. dry with materialdried over anhydrous magnesium sulphate
  7. filtrationfiltered
  8. customevaporated
  9. customThe crude product was recrystallized from isopropanol

출처 및 근거

ORD 기록
ord-9163b9084419494f9b0ad27bcb4a0fad
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08907099B2

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