Pyridine → HCID 68702137, 화합물

HRID 62016노트

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HRID 62016 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:10]=[C:11]([N+:15]([O-:17])=[O:16])[C:12]=1[O:13][CH3:14])[C:6](Cl)=NC.[N:18]1[NH:19]N=[N:21][C:22]=1[C:23]1[C:24]([C:29]([F:32])([F:31])[F:30])=[N:25][CH:26]=[CH:27][CH:28]=1.N1C=CC=C[CH:34]=1>>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:6]2[N:21]([CH3:34])[C:22]([C:23]3[C:24]([C:29]([F:32])([F:31])[F:30])=[N:25][CH:26]=[CH:27][CH:28]=3)=[N:18][N:19]=2)[CH:10]=[C:11]([N+:15]([O-:17])=[O:16])[C:12]=1[O:13][CH3:14]

참가 물질

4

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HCID 1049PyridineHCID 687044913-(2H-tetrazol-5-yl)-2-(trifluoromethyl)pyridineHCID 866431073,4-Dimethoxy-N-methyl-5-nitro-benzimidoyl chloride

생성물 1

HCID 68702137HCID 68702137, 화합물

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온도
82.5 °C

실험 절차

3,4-Dimethoxy-N-methyl-5-nitro-benzimidoyl chloride (0.28 g, 1.08 mmol) was added to a stirred solution of 3-(2H-tetrazol-5-yl)-2-(trifluoromethyl)pyridine (0.215 g, 1 mmol) in dry pyridine (3 mL), preheated to 50° C. The resulting mixture was cautiously heated to 75-90° C. and maintained at this temperature until nitrogen evolution ceased. The mixture was then poured onto water (30 mL) and extracted with dichloromethane (25 mL). The organic phase was separated, dried over anhydrous magnesium sulphate, filtered and evaporated to dryness. The resulting residue was purified by chromatography to afford 3-(5-(3,4-dimethoxy-5-nitrophenyl)-4-methyl-4H-1,2,4-triazol-3-yl)-2-(trifluoromethyl)pyridine, 0.241 g (59%).

후처리

  1. custompreheated to 50° C
  2. temperaturemaintained at this temperature until nitrogen evolution
  3. additionThe mixture was then poured onto water (30 mL)
  4. extractionextracted with dichloromethane (25 mL)
  5. customThe organic phase was separated
  6. dry with materialdried over anhydrous magnesium sulphate
  7. filtrationfiltered
  8. customevaporated to dryness
  9. customThe resulting residue was purified by chromatography

출처 및 근거

ORD 기록
ord-993bd659aac04887bd24f303e3591b9f
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09446012B2

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