化工社化工社 化学情報印刷レポート · 研究参考用
3-Bromo-2-ethoxypyridine → 5,5'-Bis[2-ethoxypyridine]
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Bromo-2-ethoxypyridine | HCID 10987308 | — |
| 触媒 | Tetraethylammonium Iodide | HCID 6225 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 触媒 | HCID 178418751 | HCID 178418751 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5,5'-Bis[2-ethoxypyridine] | HCID 824752 | — |
反応手順
The title compound was prepared as described by Constable et al.13 using NiCl2(PPh3)2 (327 mg, 0.5 mmol, 0.3 eq.), acid washed Zn powder (164 mg, 1.5 eq.) and Et4NI (435 mg, 1.7 mmol, 1 eq.) in. distilled THF (10 mL). with a solution of 5 bromo-2 ethoxypyridine (344 mg, 1.7 mmol, 1 eq.) in THF (5 mL) at 50° C. for 24 h. Workup gave a white crystalline solid (237 mg; 80%). The reaction was also carried out on a larger scale (1.0 g or 1.7 g of starting material) giving yields of 85% and 90% respectively. The spectral data were consistent with literature data13.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08748582B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-ff3335dd637e438d845ea43517055040 |
| 出典メモ | uspto-grants-2014_06 |