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2,3-Lutidine → Pyridine, 2,3-dimethyl-, 1-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,3-Lutidine | HCID 11420 | — |
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Pyridine, 2,3-dimethyl-, 1-oxide | HCID 3840573 | — |
反応手順
A solution of 24 g (0.22 mol) of 2,3-dimethylpyridine in 100 ml of methylene chloride is treated while cooling with ice with a solution of 46.6 g (0.27 mol) of m-chloroperbenzoic acid in 100 ml of methylene chloride. The reaction mixture is heated under reflux for 2 hours and concentrated in a rotary evaporator. The residue is chromatographed on silica gel with ethyl acetate/methylene chloride (3:1) as the elution agent, the medium pressure flash chromatography method being used and the pressure being produced with nitrogen gas. By recrystallization from ether there is obtained 2,3-dimethylpyridine 1-oxide of melting point 56°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04766133 |
| 出典データセット | uspto-grants-1988_08 |
| ORD ID | ord-39749d82d8984a9b830f19e45fb8b4be |
| 出典メモ | uspto-grants-1988_08 |