2-Amino-5-methylpyridine → 6-Methyl-2-[4-(trifluoromethyl)phenyl]imidazo[1,2-a]pyridine

HRID 35518

反応式

HRID 35518 の反応式
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([C:11]([F:14])([F:13])[F:12])=[CH:7][CH:6]=1)=O.[NH2:15][C:16]1[CH:21]=[CH:20][C:19]([CH3:22])=[CH:18][N:17]=1.C(=O)(O)[O-].[Na+]>C(O)C>[CH3:22][C:19]1[CH:20]=[CH:21][C:16]2[N:17]([CH:2]=[C:3]([C:5]3[CH:10]=[CH:9][C:8]([C:11]([F:14])([F:13])[F:12])=[CH:7][CH:6]=3)[N:15]=2)[CH:18]=1

参加物

5

反応物 3

HCID 153482-Amino-5-methylpyridineHCID 3219792-Bromo-4'-(trifluoromethyl)acetophenoneHCID 516892Sodium Bicarbonate

生成物 1

HCID 28138106-Methyl-2-[4-(trifluoromethyl)phenyl]imidazo[1,2-a]pyridine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

24 g (0.077 mole) of 1-bromo-2-(4-trifluoromethylphenyl)-2-ethanone, 8.4 g (0.077 mole) of 2-amino-5-methylpyridine and 13 g of sodium bicarbonate are mixed in 210 ml of 95% strength ethanol, and this suspension is heated under reflux until the evolution of gas has ceased. The solvent is then evaporated off under reduced pressure and the evaporation residue is taken up with water and dichloromethane. The organic phase is decanted and dried over magnesium sulphate, and the solvent is removed by evaporation under reduced pressure. The residue is purified by column chromatography.

後処理

  1. temperaturethis suspension is heated
  2. temperatureunder reflux until the evolution of gas
  3. customThe solvent is then evaporated off under reduced pressure
  4. customThe organic phase is decanted
  5. dry with materialdried over magnesium sulphate
  6. customthe solvent is removed by evaporation under reduced pressure
  7. customThe residue is purified by column chromatography

出典と根拠

ORDレコード
ord-a4f089c2a14f4280abf7024273451486
出典データセット
uspto-grants-1988_08
特許番号
US04767755

関連ノート

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