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Iodine chloride → 2-Chloro-5-iodopyridin-4-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodine chloride | HCID 24640 | — |
| 反応物 | 2-Chloropyridin-4-amine | HCID 84432 | — |
| 反応物 | Potassium Acetate | HCID 517044 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Chloro-5-iodopyridin-4-amine | HCID 45480366 | 40% |
反応手順
Iodine monochloride (0.758 g, 4.67 mmol) was added to a solution of 2-chloro-4-amino pyridine (0.500 g, 3.89 mmol) and potassium acetate (0.763 g, 7.78 mmol) in acetic acid (30 mL). The reaction mixture was heated under reflux for 4 hr. The solvent was removed in vacuo and the residue was partitioned between aqueous sodium hydrogenocarbonate (50 mL) and ethyl acetate (50 mL). The organic phase was dried (MgSO4) and the solvent was removed in vacuo. The crude product was purified by flash silica chromatography, eluting with ethyl acetate and hexane (1/9), to give the title compound as a pink solid (0.394 g, 40%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08367658B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-19d502a4498c4ad4971a9645883bbac5 |
| 出典メモ | uspto-grants-2013_02 |