HCID 86628083、化合物 → HCID 67037355、化合物

HRID 1401299ノート

反応式

HRID 1401299 の反応式
[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]

参加物

4

反応物 2

HCID 86628083HCID 86628083、化合物HCID 87244702HCID 87244702、化合物

生成物 1

HCID 67037355HCID 67037355、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-9163b9084419494f9b0ad27bcb4a0fad
出典データセット
uspto-grants-2014_12
特許番号
US08907099B2

反応ノート

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