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

HRID 1514156노트

반응식

HRID 1514156 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-49d082c64e524a979d4dd1170fbbaeae
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08222254B2

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