化工社化工社 化学情報印刷レポート · 研究参考用
N-bromobutanimide → Ethyl 6-(bromomethyl)picolinate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | Ethyl 6-methylpyridine-2-carboxylate | HCID 564597 | — |
| 触媒 | Benzoyl Peroxide | HCID 7187 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 生成物 | Ethyl 6-(bromomethyl)picolinate | HCID 23033755 | 98.3% |
反応手順
A mixture of 6-methyl-pyridine-2-carboxylic acid ethyl ester (1.65 g, 10 mmol), NBS (1.77 g, 10 mmol), and benzoyl peroxide (100 mg) in carbon tetrachloride (20 ml) was refluxed for 14 h. After cooling to room temperature, the reaction mixture was partitioned between diethyl ether and water (120 ml, 4:1), organic layer was washed with water (2×20 ml), brine, dried (MgSO4), filtered and concentrated to give 6-bromomethyl-pyridine-2-carboxylic acid ethyl ester (2.4 g) which was used without further purification. LCMS m/z: 245 (M+1)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07820704B2 |
| 出典データセット | uspto-grants-2010_10 |
| ORD ID | ord-68468710087740078ac5874558b61ab5 |
| 出典メモ | uspto-grants-2010_10 |