HCID 86628083, 화합물 → 5-(3,4-Dimethoxy-5-nitrophenyl)-3-(2-(trifluoromethyl)pyridin-3-yl)-1,2,4-triazine

HRID 62002노트

반응식

HRID 62002 반응식
[F:1][C:2]([F:14])([F:13])[C:3]1[N:12]=[CH:11][CH:10]=[CH:9][C:4]=1/[C:5](=[N:7]/[NH2:8])/[NH2:6].[CH3:15][O:16][C:17]1[CH:18]=[C:19]([C:28](=O)[CH:29]=O)[CH:20]=[C:21]([N+:25]([O-:27])=[O:26])[C:22]=1[O:23][CH3:24]>C(O)C>[CH3:15][O:16][C:17]1[CH:18]=[C:19]([C:28]2[N:6]=[C:5]([C:4]3[C:3]([C:2]([F:13])([F:1])[F:14])=[N:12][CH:11]=[CH:10][CH:9]=3)[N:7]=[N:8][CH:29]=2)[CH:20]=[C:21]([N+:25]([O-:27])=[O:26])[C:22]=1[O:23][CH3:24]

참가 물질

4

반응물 2

HCID 86628083HCID 86628083, 화합물HCID 87543466N'-amino-2-(trifluoromethyl)pyridine-3-carboximidamide

생성물 1

HCID 687018815-(3,4-Dimethoxy-5-nitrophenyl)-3-(2-(trifluoromethyl)pyridin-3-yl)-1,2,4-triazine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a stirred solution of (Z)-2-(trifluoromethyl)nicotinohydrazonamide (1.02 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. It was 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 5-(3,4-dimethoxy-5-nitrophenyl)-3-(2-(trifluoromethyl)pyridin-3-yl)-1,2,4-triazine, 1.628 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-042b72051a7047aea4b617ab5be8c151
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09446012B2

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