Sodium hydride → N-(2-pyridyl)-1-[2-(4-(3,4-dimethoxybenzoyl)-1-piperazinyl)ethyl]benzimidazole-2-carboxamide

HRID 476899

反応式

HRID 476899 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH:7][C:8]([C:10]1[NH:11][C:12]2[CH:18]=[CH:17][CH:16]=[CH:15][C:13]=2[N:14]=1)=[O:9].[H-].[Na+].[CH3:21][O:22][C:23]1[CH:24]=[C:25]([CH:37]=[CH:38][C:39]=1[O:40][CH3:41])[C:26]([N:28]1[CH2:33][CH2:32][N:31]([CH2:34][CH2:35]Cl)[CH2:30][CH2:29]1)=[O:27].[Cl-].[NH4+]>CS(C)=O>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH:7][C:8]([C:10]1[N:11]([CH2:35][CH2:34][N:31]2[CH2:32][CH2:33][N:28]([C:26](=[O:27])[C:25]3[CH:37]=[CH:38][C:39]([O:40][CH3:41])=[C:23]([O:22][CH3:21])[CH:24]=3)[CH2:29][CH2:30]2)[C:12]2[CH:18]=[CH:17][CH:16]=[CH:15][C:13]=2[N:14]=1)=[O:9]

参加物

6

実験手順

In an argon atmosphere, N-(2-pyridyl)benzimidazole-2-carboxamide (1.40 g) was dissolved in DMSO (20 ml), and 60% sodium hydride (0.28 g) was added and stirred at room temperature for 1 hr. A solution (7 ml) of 2-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]ethyl chloride (1.90 g) in DMSO was added dropwise and allowed to react overnight at room temperature under agitation. The reaction solution was poured into an aqueous solution of ammonium chloride and extracted with chloroform. The chloroform layer was dried over Na2SO4 and the solvent was distilled off. Purification of the residue by column chromatography on silica gel gave the title compound (1.60 g) as amorphous solid.

後処理

  1. customto react overnight at room temperature under agitation
  2. extractionextracted with chloroform
  3. dry with materialThe chloroform layer was dried over Na2SO4
  4. distillationthe solvent was distilled off
  5. customPurification of the residue by column chromatography on silica gel

出典と根拠

ORDレコード
ord-69740c2500544e618dec4d0230f5d979
出典データセット
uspto-grants-1989_12
特許番号
US04886803

関連ノート

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