化工社化工社 化学情報印刷レポート · 研究参考用
Water → 2,5-Dichloro-pyridine-3-carbaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Tributylstannane | HCID 5948 | — |
| 反応物 | 2,5-Dichloro-nicotinoyl chloride | HCID 2799996 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2,5-Dichloro-pyridine-3-carbaldehyde | HCID 21973274 | 34.4% |
反応手順
To a solution of 2,5-Dichloro-nicotinoyl chloride (15 g, 0.071 mol) in tetrahydrofuran was added tributyl-stannane (24.9 g, 0.086 mol) portionwise over 45 minutes. The resulting mixture was stirred at ambient temperature for 50 minutes, and then treated with tetrakis(triphenylphosphine)palladium(0) (0.82 g, 0.00071 mol). The reaction mixture was stirred at ambient temperature for 4 hours, poured into water; the product was extracted with ethylacetate, the combined organics were dried over magnesium sulfate, filtered and concentrated in vacuo. Silica gel chromatography (10% ethyl acetate/hexanes) followed by recrystallization from hexanes/ethylacetate gave the title compound (4.3 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07098212B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-38c6d934eb854ee7a469257bfdad0650 |
| 出典メモ | uspto-grants-2006_08 |