化工社化工社 化学情報印刷レポート · 研究参考用
Nitrogen → N-(3-(6-methoxypyridin-3-yl)-5-nitrophenyl)acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | (6-Methoxypyridin-3-yl)boronic acid | HCID 2734368 | — |
| 反応物 | N-(3-bromo-5-nitrophenyl)acetamide | HCID 10658908 | — |
| 触媒 | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | N-(3-(6-methoxypyridin-3-yl)-5-nitrophenyl)acetamide | HCID 117777422 | 81% |
反応手順
A solution of N-(3-bromo-5-nitrophenyl)acetamide (1 g, 3.86 mmol) in 1,2-dimethoxyethane (20 ml) was degassed by N2 bubbling for 5 min. (6-Methoxypyridin-3-yl)boronic acid (0.77 g, 5.0 mmol, 1.3 eq.) was added and the mixture was degassed for 5 min. Pd(dppf)Cl2 (0.630 g, 0.77 mmol, 0.2 eq.) and aqueous sodium carbonate (1.23 g, 11.58 mmol, 3.0 eq.) were added and the procedure of Example 1(d) was followed. The crude residue of the product was purified by column chromatography (60-120 silica gel, 40% ethyl acetate in hexane) to give the product in 81% yield (0.9 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09447091B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-fb6aa7ef1ade44179475dea6b4cadbe6 |
| 出典メモ | uspto-grants-2016_09 |