Sodium Iodide → HCID 22010690、化合物

HRID 323158ノート

反応式

HRID 323158 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:39]=[CH:38][C:20]([C:21]([N:23]([CH3:37])[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]Cl)=[O:22])=[CH:19][CH:18]=3)=[O:15])=[CH:10][CH:11]=[CH:12][CH:13]=2)=[CH:4][CH:3]=1.[C:40]1(=[O:50])[NH:44][C:43](=[O:45])[C:42]2=[CH:46][CH:47]=[CH:48][CH:49]=[C:41]12.[K].[I-].[Na+]>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:39]=[CH:38][C:20]([C:21]([N:23]([CH3:37])[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][N:44]4[C:43](=[O:45])[C:42]5=[CH:46][CH:47]=[CH:48][CH:49]=[C:41]5[C:40]4=[O:50])=[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 5238Sodium IodideHCID 22010757HCID 22010757、化合物HCID 24194345Phthalimide potassium salt

生成物 1

HCID 22010690HCID 22010690、化合物収率 114.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

To a solution of 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-[2-(5-chloropentyloxy)phenyl]benzamide (800 mg) in N,N-dimethylformamide (15 ml) was added Potassium phthalimide (821 mg) and sodium iodide (cat.) at ambient temperature. The reaction mixture was stirred at 80° C. for 18 hours. The reaction mixture was cooled and extracted with ethyl acetate and washed with water and brine. The organic solution was dried over magnesium sulfate. The solvent was removed by evaporation and subjected to silica gel column chromatography (SiO2; 50 g, 0.5% methanol in chloroform) to give 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-[2-(5-phthalimidopentyloxy)phenyl]benzamide (1.1 g).

後処理

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

出典と根拠

ORDレコード
ord-a7efaeac758541bca56e997da9610706
出典データセット
uspto-grants-2001_04
特許番号
US06211242B1

反応ノート

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