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

HRID 1278228

반응식

HRID 1278228 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1a3027a6c96b43e18745f0fae0541f4f
출처 데이터셋
uspto-grants-1981_07
특허 번호
US04281000

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