Pyridine → HCID 68702137、化合物

HRID 62016ノート

反応式

HRID 62016 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

HCID 68702137HCID 68702137、化合物

反応条件

温度
82.5 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-993bd659aac04887bd24f303e3591b9f
出典データセット
uspto-grants-2016_09
特許番号
US09446012B2

反応ノート

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