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

HRID 1493591

反応式

HRID 1493591 の反応式
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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7c22ef8e681e4f7a8c12840adfc4c4bf
出典データセット
uspto-grants-1991_06
特許番号
US05023258

関連ノート

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