Water → 1,2-Dihydro-6-methyl-5-(imidazo[1,2-a]pyridin-6-yl)-2-oxo-pyridine

HRID 414315

反応式

HRID 414315 の反応式
[CH3:1][C:2]1[NH:7][C:6](=[O:8])[C:5](C#N)=[CH:4][C:3]=1[C:11]1[CH:12]=[CH:13][C:14]2[N:15]([CH:17]=[CH:18][N:19]=2)[CH:16]=1.O.O.N>P(=O)(O)(O)O>[CH3:1][C:2]1[NH:7][C:6](=[O:8])[CH:5]=[CH:4][C:3]=1[C:11]1[CH:12]=[CH:13][C:14]2[N:15]([CH:17]=[CH:18][N:19]=2)[CH:16]=1

参加物

5

反応物 3

HCID 962WaterHCID 4593OlprinoneHCID 12896473Azane;hydrate

生成物 1

HCID 138523301,2-Dihydro-6-methyl-5-(imidazo[1,2-a]pyridin-6-yl)-2-oxo-pyridine収率 44.4%

試薬・触媒・溶媒 1

HCID 1004Phosphoric Acid溶媒

実験手順

In 10 ml of 85% phosphoric acid was refluxed 1 g of 1,2-dihydro-6-methyl-5-(imidazo[1,2-a]pyridin-6-yl)-2-oxo-3-pyridinecarbonitrile for 18 hours. After cooling, water was added and then conc. ammonia water was further added to the reaction mixture to render the mixture alkaline. 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 recrystallized from ethanol-ether to obtain 0.4 g of 1,2-dihydro-6-methyl-5-(imidazo[1,2-a]pyridin-6-yl)-2-oxo-pyridine.

後処理

  1. temperatureAfter cooling
  2. extractionThe mixture was extracted with chloroform
  3. washAfter washing with water
  4. dry with materialdrying over magnesium sulfate, chloroform
  5. customwas removed by distillation under reduced pressure
  6. customThe residue was recrystallized from ethanol-ether

出典と根拠

ORDレコード
ord-deaf50ac95c54fa5b029f10b0eaf4181
出典データセット
uspto-grants-1988_12
特許番号
US04791202

関連ノート

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