Potassium Carbonate → HCID 22010632、化合物

HRID 323157ノート

反応式

HRID 323157 の反応式
[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

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 531671-MethylpiperazineHCID 22010658HCID 22010658、化合物

生成物 1

HCID 22010632HCID 22010632、化合物収率 33.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-62f8cb90fb524b10929c47551b172df2
出典データセット
uspto-grants-2001_04
特許番号
US06211242B1

反応ノート

読み込み中…