Methyl iodide → HCID 178503348、化合物

HRID 587493ノート

反応式

HRID 587493 の反応式
[NH:1]1[C:9]2[C:4](=[N:5][CH:6]=[CH:7][CH:8]=2)[N:3]=[C:2]1[SH:10].CI.[C:13]([O-])([O-])=O.[K+].[K+]>CC(C)=O>[CH3:13][S:10][C:2]1[NH:3][C:4]2=[N:5][CH:6]=[CH:7][CH:8]=[C:9]2[N:1]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 178527819HCID 178527819、化合物

生成物 1

HCID 178503348HCID 178503348、化合物収率 45.8%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of 1H-imidazo[4,5-b]pyridine-2-thiol (2 g) in acetone (30 mL) were added MeI (0.910 mL) and K2CO3 (5.48 g) at room temperature. After stirring for 10 h, the mixture was concentrated under reduced pressure. The residue was purified by column chromatography (NH-silica gel, eluted with 10%-100% EtOAc in hexane) to give 2-(methylsulfanyl)-3H-imidazo[4,5-b]pyridine (1.0 g) as a white solid.

後処理

  1. concentrationthe mixture was concentrated under reduced pressure
  2. customThe residue was purified by column chromatography (NH-silica gel, eluted with 10%-100% EtOAc in hexane)

出典と根拠

ORDレコード
ord-92fa7ad1de724315966070998af52654
出典データセット
uspto-grants-2016_01
特許番号
US09226921B2

反応ノート

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