Potassium Carbonate → HCID 22010632, 화합물

HRID 323157노트

반응식

HRID 323157 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:37]=[CH:36][C:20]([C:21]([N:23]([CH3:35])[C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=4[O:30][CH2:31][CH2:32][CH2:33]Br)=[O:22])=[CH:19][CH:18]=3)=[O:15])=[CH:10][CH:11]=[CH:12][CH:13]=2)=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:44][N:45]1[CH2:50][CH2:49][NH:48][CH2:47][CH2:46]1>CN(C)C=O>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]([C:14]([NH:16][C:17]3[CH:37]=[CH:36][C:20]([C:21]([N:23]([CH3:35])[C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=4[O:30][CH2:31][CH2:32][CH2:33][N:48]4[CH2:49][CH2:50][N:45]([CH3:44])[CH2:46][CH2:47]4)=[O:22])=[CH:19][CH:18]=3)=[O:15])=[CH:10][CH:11]=[CH:12][CH:13]=2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 531671-MethylpiperazineHCID 22010658HCID 22010658, 화합물

생성물 1

HCID 22010632HCID 22010632, 화합물수율 33.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

To a solution of 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-[2-(3-bromopropoxy)phenyl]benzamide (520 mg) in N,N-dimethylformamide (15 ml) was added potassium carbonate (386 mg) and 1-methylpiperazine (280 mg) at ambient temperature. The reaction mixture was stirred at 60° C. for 12 hours. The reaction mixture was cooled and extracted with ethyl acetate and washed with water, 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, 10% methanol in chloroform) to give 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-[2-[3-(4-methylpiperazin-1-yl)propoxy]phenyl]benzamide (180 mg).

후처리

  1. temperatureThe reaction mixture was cooled
  2. extractionextracted with ethyl acetate
  3. washwashed with water, 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-62f8cb90fb524b10929c47551b172df2
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211242B1

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