Phenyl isocyanate → 2-{3-[4-(2-Methoxyphenyl)piperazino]propanoyl}-N-phenyl-1-hydrazinecarboxamide

HRID 1514156ノート

反応式

HRID 1514156 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][C:17]([NH:19][NH2:20])=[O:18])[CH2:11][CH2:10]1.[C:21]1([N:27]=[C:28]=[O:29])[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:10][CH2:11][N:12]([CH2:15][CH2:16][C:17]([NH:19][NH:20][C:28]([NH:27][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[O:29])=[O:18])[CH2:13][CH2:14]1

参加物

4

反応物 2

HCID 7672Phenyl isocyanateHCID 8724333-[4-(2-Methoxyphenyl)piperazino]propanohydrazide

生成物 1

HCID 595364632-{3-[4-(2-Methoxyphenyl)piperazino]propanoyl}-N-phenyl-1-hydrazinecarboxamide収率 83.9%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a suspension of 3-[4-(2-methoxyphenyl)piperazino]propanohydrazide D2 (1.00 g, 3.60 mmol) in anhydrous toluene (2 mL), phenyl isocyanate (0.45 g, 0.41 mL, 3.78 mmol) was added and the mixture was stirred at room temperature for 30 min and then heated at reflux for 1 h. The solution was allowed to cool slowly to room temperature and the resulting precipitate was filtered and washed with hexane to afford 1.2 g (83.9%) 2-{3-[4-(2-methoxyphenyl)piperazino]propanoyl}-N-phenyl-1-hydrazinecarboxamide D5 as a white solid.

後処理

  1. additionwas added
  2. temperatureheated
  3. temperatureat reflux for 1 h
  4. temperatureto cool slowly to room temperature
  5. filtrationthe resulting precipitate was filtered
  6. washwashed with hexane

出典と根拠

ORDレコード
ord-49d082c64e524a979d4dd1170fbbaeae
出典データセット
uspto-grants-2012_07
特許番号
US08222254B2

反応ノート

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