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Sodium Iodide → Methyl 2-iodoisonicotinate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Methyl Ethyl Ketone | HCID 6569 | — |
| 反応物 | 2-Chloroisonicotinic acid | HCID 236985 | — |
| 生成物 | Methyl 2-iodoisonicotinate | HCID 196869 | 92.4% |
反応手順
A solution of 2-chloro-pyridine-4-carboxylic acid (5 g, 31.7 mmol) in butan-2-one (150 ml) was heated under reflux with sodium iodide for 6 h to afford the 2-iodo-isonicotinic acid (7.3 g, 92.4% yield) following extractive aqueous workup. This material was dissolved in THF (50 ml) and esterified with fresh etheral diazomethane solution (44 ml, 0.55 mol/l). After evaporation of the solvent and filtration through a pad of silica gel, [elution with CH2Cl2/(2M NH3 MeOH)=19:1] the title compound (2.3 g, 44%) was obtained as a dark yellow oil. MS: m/e=263.0 (M1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06610723B2 |
| 出典データセット | uspto-grants-2003_08 |
| ORD ID | ord-d023fd732fc2496ea42b4ea746578c81 |
| 出典メモ | uspto-grants-2003_08 |