Methyl iodide → HCID 69239194, 화합물

HRID 1295773노트

반응식

HRID 1295773 반응식
[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]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 86589517HCID 86589517, 화합물

생성물 1

HCID 69239194HCID 69239194, 화합물수율 95%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-dfcd99def99b4a9aacb17355d7086cff
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07244744B2

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