Potassium Carbonate → 1-(4-Methoxyphenyl)-4-(5-nitro-2-pyridinyl)piperazine

HRID 1493591

반응식

HRID 1493591 반응식
Cl.Cl.[CH3:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([N:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)=[CH:7][CH:6]=1.Cl[C:18]1[CH:23]=[CH:22][C:21]([N+:24]([O-:26])=[O:25])=[CH:20][N:19]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.O>[CH3:3][O:4][C:5]1[CH:6]=[CH:7][C:8]([N:11]2[CH2:16][CH2:15][N:14]([C:18]3[CH:23]=[CH:22][C:21]([N+:24]([O-:26])=[O:25])=[CH:20][N:19]=3)[CH2:13][CH2:12]2)=[CH:9][CH:10]=1

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 783082-Chloro-5-nitropyridineHCID 27237001-(4-Methoxyphenyl)-piperazine, dihydrochloride

생성물 1

HCID 37426761-(4-Methoxyphenyl)-4-(5-nitro-2-pyridinyl)piperazine

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A mixture of 1-(4-methoxyphenyl)piperazine dihydrochloride (5.30 g, 20 mmole), 2-chloro-5-nitropyridine (3.2 g, 20 mmole) and potassium carbonate (4.14 g, 30 mmole) in DMF (20 ml) was heated at 120° for 66 hours. The reaction mixture was cooled, diluted with water and the resulting precipitate collected by filtration. To this solid was added methanol (200 ml) and the mixture was heated under reflux for 0.17 hour. After cooling, the solid was collected by filtration and dried to yield the desired product, m.p. 165°-6° (4.0 g, 64%), which was used without further purification.

후처리

  1. temperaturewas heated at 120° for 66 hours
  2. temperatureThe reaction mixture was cooled
  3. filtrationthe resulting precipitate collected by filtration
  4. additionTo this solid was added methanol (200 ml)
  5. temperaturethe mixture was heated
  6. temperatureunder reflux for 0.17 hour
  7. temperatureAfter cooling
  8. filtrationthe solid was collected by filtration
  9. customdried

출처 및 근거

ORD 기록
ord-7c22ef8e681e4f7a8c12840adfc4c4bf
출처 데이터셋
uspto-grants-1991_06
특허 번호
US05023258

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