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2-Pyridinamine, N-methyl- → (5-Iodo-pyridin-2-yl)-methyl-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Pyridinamine, N-methyl- | HCID 20727 | — |
| 反応物 | Sodium Sulfite | HCID 24437 | — |
| 反応物 | Iodine chloride | HCID 24640 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (5-Iodo-pyridin-2-yl)-methyl-amine | HCID 11253290 | 62% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08497260B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-b0631fd8e3884387aee95925ef8722a4 |
| 出典メモ | uspto-grants-2013_07 |