1-(3-Pyridyl)-3-(dimethylamino)-2-propen-1-one → Phenyl[7-(3-pyridinyl)pyrazolo[1,5-a]pyrimidin-3-yl]methanone

HRID 1247945

反応式

HRID 1247945 の反応式
[NH2:1][C:2]1[C:6]([C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[O:8])=[CH:5][NH:4][N:3]=1.CN(C)[CH:17]=[CH:18][C:19]([C:21]1[CH:22]=[N:23][CH:24]=[CH:25][CH:26]=1)=O>C(O)(=O)C>[C:9]1([C:7]([C:6]2[CH:5]=[N:4][N:3]3[C:19]([C:21]4[CH:22]=[N:23][CH:24]=[CH:25][CH:26]=4)=[CH:18][CH:17]=[N:1][C:2]=23)=[O:8])[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

参加物

4

反応物 2

HCID 5670331-(3-Pyridyl)-3-(dimethylamino)-2-propen-1-oneHCID 178509267HCID 178509267、化合物

生成物 1

HCID 13475883Phenyl[7-(3-pyridinyl)pyrazolo[1,5-a]pyrimidin-3-yl]methanone

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A reaction mixture of 1.87 g of (3-amino-1H-pyrazol-4-yl)phenyl-methanone and 1.76 g of 3-dimethylamino-1-(3-pyridinyl)-2-propen-1-one in 25 ml of glacial acetic acid was refluxed for 6 hours and then the solvent was removed in vacuo giving a crystalline residue. This residue was partitioned between saturated aqueous sodium bicarbonate and methylene chloride. The organic layer was dried with anhydrous sodium sulfate and then passed through a short pad of hydrous magnesium silicate. The addition of hexane to the refluxing eluate induced crystallization. After cooling, the desired product was collected, giving 2.45 g, mp 202°-203° C.

後処理

  1. temperaturewas refluxed for 6 hours
  2. customthe solvent was removed in vacuo
  3. customgiving a crystalline residue
  4. customThis residue was partitioned between saturated aqueous sodium bicarbonate and methylene chloride
  5. dry with materialThe organic layer was dried with anhydrous sodium sulfate
  6. additionThe addition of hexane
  7. customto the refluxing eluate induced crystallization
  8. temperatureAfter cooling
  9. customthe desired product was collected
  10. customgiving 2.45 g, mp 202°-203° C.

出典と根拠

ORDレコード
ord-6b10309a69b94dc7b98e385b4534211e
出典データセット
uspto-grants-1985_06
特許番号
US04521422

関連ノート

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