Hydrochloric Acid → 1-(Imidazo[1,2-a]pyridin-6-yl)propan-2-one

HRID 579966

反応式

HRID 579966 の反応式
[N+]([C:4]([CH3:15])=[CH:5][C:6]1[CH:7]=[CH:8][C:9]2[N:10]([CH:12]=[CH:13][N:14]=2)[CH:11]=1)([O-])=O.Cl.[OH2:17]>CCO>[N:14]1[CH:13]=[CH:12][N:10]2[CH:11]=[C:6]([CH2:5][C:4](=[O:17])[CH3:15])[CH:7]=[CH:8][C:9]=12

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 539155686-(2-Nitro-1-propenyl)imidazo[1,2-a]pyridine

生成物 1

HCID 138523111-(Imidazo[1,2-a]pyridin-6-yl)propan-2-one

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In 25 ml of water and 25 ml of EtOH, 1.14 g of 6-(2-nitro-1-propenyl)imidazo[1,2-a]pyridine was heated to 80° C. together with 100 mg of ferrous chloride. With stirring, 2.5 ml of conc. hydrochloric acid was added at a refluxing rate and the mixture was stirred of 1 hour. Upon heating, insoluble matter was removed by filtration. After the insoluble matter was thoroughly washed with ethanol, the solvent was removed by distillation under reduced pressure. An aqueous sodium bicarbonate solution was added to the residue and the mixture was extracted with chloroform. After washing with water and drying over magnesium sulfate, chloroform was removed by distillation under reduced pressure. The residue was purified by column chromatography to obtain 500 mg of 1-(imidazo[1,2-a]pyridin-6-yl)-2-propanone.

後処理

  1. stirringthe mixture was stirred of 1 hour
  2. temperatureUpon heating
  3. custominsoluble matter was removed by filtration
  4. washAfter the insoluble matter was thoroughly washed with ethanol
  5. customthe solvent was removed by distillation under reduced pressure
  6. additionAn aqueous sodium bicarbonate solution was added to the residue
  7. extractionthe mixture was extracted with chloroform
  8. washAfter washing with water
  9. dry with materialdrying over magnesium sulfate, chloroform
  10. customwas removed by distillation under reduced pressure
  11. customThe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-322725c5bea54e23b380427b1df4f5b1
出典データセット
uspto-grants-1988_06
特許番号
US04751227

関連ノート

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