化工社化工社 化学情報印刷レポート · 研究参考用
m-Chloroperbenzoic acid → 2-Chloro-4-methylpyridine 1-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | 2-Chloro-4-methylpyridine | HCID 77248 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2-Chloro-4-methylpyridine 1-oxide | HCID 12487484 | 464.3% |
反応手順
40% meta-chloroperbenzoic acid (13.5 g, 31.4 mmol) was added at ambient temperature to a solution of 2-chloro-4-methyl-pyridine (2.0 g, 1.5 mmol) in chloroform (20 mL) and heated at reflux for 24 h. After allowing to cool, the mixture was washed with water followed by sodium bicarbonate solution. The separated organic phase was further washed with water and brine, dried over anhydrous sodium sulfate and concentrated to give a residue which was purified by column chromatography over silica gel (60-120 mesh) using 10% methanol in ethyl acetate as eluent to afford 2-chloro-4-methyl-pyridine 1-oxide (1.0 g, 45%) as a deep brown oily liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08524705B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-c2ddec53bd744cd7b5a933c42f3d5d64 |
| 出典メモ | uspto-grants-2013_09 |