Methyl iodide → HCID 69239194、化合物

HRID 1295773ノート

反応式

HRID 1295773 の反応式
[CH2:1]([C:5]1[CH:10]=[CH:9][C:8]([C:11]([N:13]2[CH2:18][CH2:17][CH:16]([N:19]3[C:23]4[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=4[NH:21][C:20]3=[S:28])[CH2:15][CH2:14]2)=[O:12])=[CH:7][CH:6]=1)[CH2:2][CH2:3][CH3:4].CI.[C:31](=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH2:1]([C:5]1[CH:6]=[CH:7][C:8]([C:11]([N:13]2[CH2:18][CH2:17][CH:16]([N:19]3[C:23]4[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=4[N:21]=[C:20]3[S:28][CH3:31])[CH2:15][CH2:14]2)=[O:12])=[CH:9][CH:10]=1)[CH2:2][CH2:3][CH3:4]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 86589517HCID 86589517、化合物

生成物 1

HCID 69239194HCID 69239194、化合物収率 95%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of (4-butyl-phenyl)-[4-(2-thioxo-2,3-dihydro-benzoimidazol-1-yl)-piperidin-1-yl]-methanone (0.167 g, 0.424 mmol) in acetonitrile (5 mL) was treated with methyl iodide (0.120 g, 0.848 mmol) and potassium carbonate (0.117 g, 0.848 mmol). The reaction mixture was stirred 18 h then filtered and concentrated under reduced pressure. The crude product was purified by column chromatography on silica gel using ethyl acetate as the eluent to give (4-butyl-phenyl)-[4-(2-methylsulfanyl-benzoimidazol-1-yl)-piperidin-1-yl]-methanone (0.164 g; 95%).

後処理

  1. filtrationthen filtered
  2. concentrationconcentrated under reduced pressure
  3. customThe crude product was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-dfcd99def99b4a9aacb17355d7086cff
出典データセット
uspto-grants-2007_07
特許番号
US07244744B2

反応ノート

読み込み中…