3-amino-5-methyl-1H-pyrazole-4-carbonitrile → 2-Methyl-7-(3-pyridyl)pyrazolo[1,5-a]pyrimidine-3-carbonitrile

HRID 1278228

反応式

HRID 1278228 の反応式
C[N:2]([CH3:13])[CH:3]=[CH:4][C:5]([C:7]1[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=1)=O.[NH2:14][C:15]1[C:19](C#N)=[C:18]([CH3:22])[NH:17][N:16]=1>C(O)(=O)C>[CH3:22][C:18]1[C:19]([C:15]#[N:14])=[C:13]2[N:2]=[CH:3][CH:4]=[C:5]([C:7]3[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=3)[N:16]2[N:17]=1

参加物

4

反応物 2

HCID 2274603-amino-5-methyl-1H-pyrazole-4-carbonitrileHCID 5670331-(3-Pyridyl)-3-(dimethylamino)-2-propen-1-one

生成物 1

HCID 112648292-Methyl-7-(3-pyridyl)pyrazolo[1,5-a]pyrimidine-3-carbonitrile

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 3.50 g. of 3-dimethylamino-1-(3-pyridyl)-2-propen-1-one, 25 L ml. of glacial acetic acid and 2.44 g. of 3-amino-5-methylpyrazole-4-carbonitrile is refluxed 6 hours. The solvent is removed in vacuo. The residue is dissolved in dichloromethane and the solution washed with saturated sodium bicarbonate solution. The dichloromethane layer is dried over anhydrous sodium sulfate and pased through a column of hydrous magnesium silicate. The eluent is concentrated and hexane added to give 2.60 g. of the product of the example, m.p. 245°-246° C.

後処理

  1. additionA mixture of 3.50 g
  2. customThe solvent is removed in vacuo
  3. dissolutionThe residue is dissolved in dichloromethane
  4. washthe solution washed with saturated sodium bicarbonate solution
  5. dry with materialThe dichloromethane layer is dried over anhydrous sodium sulfate
  6. concentrationThe eluent is concentrated
  7. additionhexane added
  8. customto give 2.60 g

出典と根拠

ORDレコード
ord-1a3027a6c96b43e18745f0fae0541f4f
出典データセット
uspto-grants-1981_07
特許番号
US04281000

関連ノート

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