1-Methylpiperazine → HCID 22010655, 화합물

HRID 323160노트

반응식

HRID 323160 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]([C:14]([NH:16][C:17]3[CH:48]=[CH:47][C:20]([C:21]([N:23]([CH3:46])[C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=4[O:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][NH:36][C:37]([O:39]C4C=CC=CC=4)=O)=[O:22])=[CH:19][CH:18]=3)=[O:15])=[CH:10][CH:11]=[CH:12][CH:13]=2)=[CH:4][CH:3]=1.[CH3:49][N:50]1[CH2:55][CH2:54][NH:53][CH2:52][CH2:51]1>CN(C)C=O>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:9]([C:14]([NH:16][C:17]3[CH:18]=[CH:19][C:20]([C:21]([N:23]([CH3:46])[C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=4[O:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][NH:36][C:37]([N:53]4[CH2:54][CH2:55][N:50]([CH3:49])[CH2:51][CH2:52]4)=[O:39])=[O:22])=[CH:47][CH:48]=3)=[O:15])=[CH:10][CH:11]=[CH:12][CH:13]=2)=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 531671-MethylpiperazineHCID 22010872HCID 22010872, 화합물

생성물 1

HCID 22010655HCID 22010655, 화합물수율 64.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

To a solution of 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-[2-(5-phenoxycarbonylaminopentyloxy)phenyl]benzamide (290 mg) in N,N-dimethylformamide (15 ml) was added 1-methylpiperazine (271 mg) at ambient temperature. The reaction mixture was stirred at 80° C. for 10 hours. The reaction mixture was cooled and extracted with ethyl acetate and washed with saturated sodium hydrogen carbonate and brine. The organic solution was dried over sodium sulfate. The solvent was removed by evaporation and subjected to silica gel column chromatography (SiO2; 30 g, 5% methanol in chloroform) to give 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-[2-[5-(4-methylpiperazin-1-carbonylamino)pentyloxy]phenyl]benzamide (190 mg).

후처리

  1. temperatureThe reaction mixture was cooled
  2. extractionextracted with ethyl acetate
  3. washwashed with saturated sodium hydrogen carbonate and brine
  4. dry with materialThe organic solution was dried over sodium sulfate
  5. customThe solvent was removed by evaporation

출처 및 근거

ORD 기록
ord-0e94d22493fb4be4a746d2d960776626
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211242B1

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