(Isocyanatomethyl)cyclohexane → N-(Cyclohexylmethyl)-2-{3-[4-(3-nitrophenyl)piperazin-1-yl]propanoyl}hydrazine carboxamide

HRID 1514159노트

반응식

HRID 1514159 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([N:10]2[CH2:15][CH2:14][N:13]([CH2:16][CH2:17][C:18]([NH:20][NH2:21])=[O:19])[CH2:12][CH2:11]2)[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].[CH2:22]1[CH2:27][CH2:26][CH:25]([CH2:28][N:29]=[C:30]=[O:31])[CH2:24][CH2:23]1>C1(C)C=CC=CC=1>[CH:25]1([CH2:28][NH:29][C:30]([NH:21][NH:20][C:18](=[O:19])[CH2:17][CH2:16][N:13]2[CH2:14][CH2:15][N:10]([C:6]3[CH:7]=[CH:8][CH:9]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=3)[CH2:11][CH2:12]2)=[O:31])[CH2:26][CH2:27][CH2:22][CH2:23][CH2:24]1

참가 물질

4

반응물 2

HCID 3414518(Isocyanatomethyl)cyclohexaneHCID 595364643-[4-(3-Nitrophenyl)piperazino]propanohydrazide

생성물 1

HCID 59536466N-(Cyclohexylmethyl)-2-{3-[4-(3-nitrophenyl)piperazin-1-yl]propanoyl}hydrazine carboxamide수율 95%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
70 °C

실험 절차

A solution of 3-[4-(3-nitrophenyl)piperazino]propanohydrazide D7 (0.55 g, 1.87 mmol) in toluene (30 mL) was heated at 70° C. and cyclohexanemethyl isocyanate (0.28 g, 0.30 mL, 1.96 mmol) was added at once. The slurry was heated at 70° C. until all solid went into solution (15 min) and then cooled to room temperature. The resulting solid was filtered and washed with toluene to afford 0.70 g (95%) N-(cyclohexylmethyl)-2-{3-[4-(3-nitrophenyl)piperazin-1-yl]propanoyl}hydrazine carboxamide D8 as an orange semi-solid.

후처리

  1. customwent into solution (15 min)
  2. temperaturecooled to room temperature
  3. filtrationThe resulting solid was filtered
  4. washwashed with toluene

출처 및 근거

ORD 기록
ord-3eedda883b314a1db244a6f58d6f3ea2
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08222254B2

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