2-(Methylthio)benzimidazole → 1-{[2-(methylthio)-1H-benzimidazol-1-yl]methyl}-4-propylpyrrolidin-2-one

HRID 1295817

反応式

HRID 1295817 の反応式
C(N(CC)C(=O)O[CH2:6][N:7]1[CH2:11][CH:10]([CH2:12][CH2:13][CH3:14])[CH2:9][C:8]1=[O:15])C.[CH3:19][S:20][C:21]1[NH:22][C:23]2[CH:29]=[CH:28][CH:27]=[CH:26][C:24]=2[N:25]=1>C(#N)C>[CH3:19][S:20][C:21]1[N:22]([CH2:6][N:7]2[CH2:11][CH:10]([CH2:12][CH2:13][CH3:14])[CH2:9][C:8]2=[O:15])[C:23]2[CH:29]=[CH:28][CH:27]=[CH:26][C:24]=2[N:25]=1

参加物

4

反応物 2

HCID 235392-(Methylthio)benzimidazoleHCID 11448237(2-Oxo-4-propylpyrrolidin-1-yl)methyl diethylcarbamate

生成物 1

HCID 111508421-{[2-(methylthio)-1H-benzimidazol-1-yl]methyl}-4-propylpyrrolidin-2-one収率 40.3%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of (2-oxo-4-propylpyrrolidin-1-yl)methyl diethylcarbamate a26 (1 eq, 3.18 mmol, 0.5 g) and 2-(methylthio)-benzimidazole (1.25 eq, 3.90 mmol, 0.64 g) in acetonitrile (4 ml) was heated under reflux for 42 h. The solvent was evaporated under reduce pressure and purification by preparative chromatography on reverse phase afforded 390 mg of 1-{[2-(methylthio)-1H-benzimidazol-1-yl]methyl}-4-propylpyrrolidin-2-one 90 (HPLC purity (U.V.): 85%; Yield: 40.3%).

後処理

  1. temperatureunder reflux for 42 h
  2. customThe solvent was evaporated
  3. custompressure and purification by preparative chromatography on reverse phase

出典と根拠

ORDレコード
ord-ec4a7afc21ab4e00a3bd9ec8f4ba32d4
出典データセット
uspto-grants-2007_07
特許番号
US07244747B2

関連ノート

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