化工社化工社 化学情報印刷レポート · 研究参考用
Pyridine → N-(4-chloropyridin-3-yl)-2-nitrobenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 2-Nitrobenzoyl chloride | HCID 11875 | — |
| 反応物 | 3-Amino-4-chloropyridine | HCID 581932 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-(4-chloropyridin-3-yl)-2-nitrobenzamide | HCID 67434091 | — |
反応手順
A solution of 3-amino-4-chloropyridine (5 g, 39 mmol), 2-nitrobenzoyl chloride (5.1 mL, 39 mmol) and pyridine (11 mL) in tetrahydrofuran (50 mL) was stirred for 20 hours. The reaction mixture was partitioned between water (200 mL) and dichloromethane (600 mL). The phases were separated and the organic phase was washed with water (150 mL) then brine (150 mL). The organic phase was dried over sodium sulfate, filtered and concentrated in vacuo. The crude product was purified by flash chromatography (SiO2, 10% ethyl acetate in dichloromethane). The N-(4-chloropyridin-3-yl)-2-nitrobenzamide was obtained as a brown solid (2.0 g). LCMS [M+H]: 279.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541407B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-fa642dc6671442b284ddd57048d9fa5b |
| 出典メモ | uspto-grants-2013_09 |