Hexane → N-(Cyclohexylmethyl)-2-{3-[4-(2-methoxyphenyl)piperazino]propanoyl}-1-hydrazinecarboxamide

HRID 1514155노트

반응식

HRID 1514155 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.[CH2:21]1[CH2:26][CH2:25][CH:24]([CH2:27][N:28]=[C:29]=[O:30])[CH2:23][CH2:22]1.CCCCCC>C1(C)C=CC=CC=1>[CH:24]1([CH2:27][NH:28][C:29]([NH:20][NH:19][C:17](=[O:18])[CH2:16][CH2:15][N:12]2[CH2:11][CH2:10][N:9]([C:4]3[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=3[O:2][CH3:1])[CH2:14][CH2:13]2)=[O:30])[CH2:25][CH2:26][CH2:21][CH2:22][CH2:23]1

참가 물질

5

반응물 3

HCID 8058HexaneHCID 872433HCID 872433, 화합물HCID 3414518(Isocyanatomethyl)cyclohexane

생성물 1

HCID 59536472N-(Cyclohexylmethyl)-2-{3-[4-(2-methoxyphenyl)piperazino]propanoyl}-1-hydrazinecarboxamide수율 87%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a suspension of 3-[4-(2-methoxyphenyl)piperazino]propanohydrazide D2 (0.30 g, 1.07 mmol) in anhydrous toluene (5 mL), cyclohexanemethyl isocyanate (0.16 g, 0.165 mL, 1.16 mmol) was added and the mixture was heated at reflux until all solid dissolved. The solution was allowed to cool slowly to room temperature. Hexane was added and the resulting oil was extracted with ethyl acetate, the organic phase was washed with water, dried over MgSO4 and evaporated under reduced pressure to afford 0.40 mg (87%) N-(cyclohexylmethyl)-2-{3-[4-(2-methoxyphenyl)piperazino]propanoyl}-1-hydrazinecarboxamide D4 as a pale yellow oil.

후처리

  1. additionwas added
  2. temperaturethe mixture was heated
  3. temperatureat reflux until all solid
  4. dissolutiondissolved
  5. extractionthe resulting oil was extracted with ethyl acetate
  6. washthe organic phase was washed with water
  7. dry with materialdried over MgSO4
  8. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-b91fa6dd1a93457f8d20718ee95a200b
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08222254B2

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