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

HRID 2230098
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HRID 2230098 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-ce9e58261ca84e85951547e0d8d23109
출처 데이터셋
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06423716B1

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