2-Pyridinamine, N-methyl- → (5-Iodo-pyridin-2-yl)-methyl-amine

HRID 454808

反応式

HRID 454808 の反応式
[CH3:1][NH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1.[I:9]Cl.S([O-])([O-])=O.[Na+].[Na+]>ClCCl>[CH3:1][NH:2][C:3]1[CH:8]=[CH:7][C:6]([I:9])=[CH:5][N:4]=1

参加物

5

反応物 3

HCID 207272-Pyridinamine, N-methyl-HCID 24437Sodium SulfiteHCID 24640Iodine chloride

生成物 1

HCID 11253290(5-Iodo-pyridin-2-yl)-methyl-amine収率 62%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

2-(N-Monomethylamino)pyridine (98, 1.00 g, 5.55 mmol) was dissolved in dichloromethane (20 mL) and a 1 M iodine monochloride (ICl, 6.10 mL, 6.10 mmol) dichloromethane solution was slowly added at 0° C., and stirred for 30 minutes. To the reaction mixture was added a 10% aqueous solution of sodium sulfite (Na2S2O3) and organic compounds were extracted with dichloromethane and evaporated after a treatment with sodium sulfate. Purification was performed by column chromatograph to give the target compound 2-(N-monomethylamino)-5-iodopyridine (99, 800 mg, 62%) as a yellow solid.

後処理

  1. extractionwere extracted with dichloromethane
  2. customevaporated after a treatment with sodium sulfate
  3. customPurification

出典と根拠

ORDレコード
ord-b0631fd8e3884387aee95925ef8722a4
出典データセット
uspto-grants-2013_07
特許番号
US08497260B2

関連ノート

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