Methyl iodide → 2-(2-ethylsulfanyl-phenyl)-3-methyl-6-methylsulfanyl-3H-imidazo[4,5-b]pyridine

HRID 533637ノート

反応式

HRID 533637 の反応式
[CH2:1]([S:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]1[N:19]([CH3:20])[C:13]2=[N:14][CH:15]=[C:16]([SH:18])[CH:17]=[C:12]2[N:11]=1)[CH3:2].I[CH3:22].[OH-].[K+].[Cl-].[NH4+]>C(O)C>[CH2:1]([S:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]1[N:19]([CH3:20])[C:13]2=[N:14][CH:15]=[C:16]([S:18][CH3:22])[CH:17]=[C:12]2[N:11]=1)[CH3:2]

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 14797Potassium HydroxideHCID 25517Ammonium ChlorideHCID 680912052-(2-ethylsulfanyl-phenyl)-3-methyl-3H-imidazo[4,5-b]pyridin-6-thiol

生成物 1

HCID 680912082-(2-ethylsulfanyl-phenyl)-3-methyl-6-methylsulfanyl-3H-imidazo[4,5-b]pyridine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a mixture of 2-(2-ethylsulfanyl-phenyl)-3-methyl-3H-imidazo[4,5-b]pyridin-6-thiol (535 mg), iodomethane (166 μl), and ethanol (5 ml), potassium hydroxide (200 mg) was added at room temperature, and stirred for 5 hours. To the reaction mixture, saturated aqueous ammonium chloride solution was added, and extracted with ethyl acetate. The combined organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 515 mg of 2-(2-ethylsulfanyl-phenyl)-3-methyl-6-methylsulfanyl-3H-imidazo[4,5-b]pyridine (hereinafter referred to as Present Compound 253).

後処理

  1. additionwas added at room temperature
  2. extractionextracted with ethyl acetate
  3. dry with materialThe combined organic layer was dried over sodium sulfate
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-1bc18950244a4789b452b81859b2214b
出典データセット
uspto-grants-2014_10
特許番号
US08853238B2

反応ノート

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