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Piperazine → 1-Methyl-4-(1-piperazinyl)-1H-pyrazolo[3,4-d]pyrimidine

HRID 2230098
ノート
印刷プレビュー

反応式

HRID 2230098 の反応式
Cl[C:2]1[N:7]=[CH:6][N:5]=[C:4]2[N:8]([CH3:11])[N:9]=[CH:10][C:3]=12.OC1N=CN=C2N(C)N=CC=12.[NH:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1>C(O)(C)C>[CH3:11][N:8]1[C:4]2=[N:5][CH:6]=[N:7][C:2]([N:23]3[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]3)=[C:3]2[CH:10]=[N:9]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 4837PiperazineHCID 2197514-chloro-1-methyl-1H-pyrazolo(3,4-d)pyrimidineHCID 178481767HCID 178481767、化合物

生成物 1

HCID 113564151-Methyl-4-(1-piperazinyl)-1H-pyrazolo[3,4-d]pyrimidine収率 83%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

According to the method described in J. Org. Chem., 21: 1240-1256 (1956), 4-chloro-1-methyl-1H-pyrazolo[3,4-d]pyrimidine was derived from 4-hydroxy-1-methyl-1H-pyrazolo[3,4-d]pyrimidine (1.20 g, 8.03 mmol). To this partially purified product, an isopropanol solution (50 mL) of piperazine (5.55 g, 64.4 mmol) was added, followed by stirring at room temperature for 1 hour and then heating under reflux for 1 hour. The reaction solution was concentrated, saturated brine was added thereto, the mixture was extracted with chloroform, the extract was washed with saturated brine and dried over anhydrous sodium sulfate, and then the solvent was evaporated to give the target compound (1.44 g, 6.61 mmol).

後処理

  1. temperatureheating
  2. temperatureunder reflux for 1 hour
  3. concentrationThe reaction solution was concentrated
  4. additionsaturated brine was added
  5. extractionthe mixture was extracted with chloroform
  6. washthe extract was washed with saturated brine
  7. dry with materialdried over anhydrous sodium sulfate
  8. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-ce9e58261ca84e85951547e0d8d23109
出典データセット
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06423716B1

反応ノート

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