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m-Chloroperbenzoic acid → 2-(4-methylphenyl)-6-methylpyridine-N-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-Methyl-6-(4-methylphenyl)pyridine | HCID 603081 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2-(4-methylphenyl)-6-methylpyridine-N-oxide | HCID 19430330 | 57.2% |
反応手順
A solution of 2-(4-methylphenyl)-6-methylpyridine (4.5 g) in 100 ml of chloroform was cooled to 0° C., and m-chloroperbenzoic acid (7.7 g) in 50 ml of chloroform was added over a period of 15 minutes. The mixture was stirred at room temperature for 3 hours, then at 50° C. for 2 hours, followed by stirring overnight at room temperature. Solvent was evaporated to a small volume under reduced pressure, and the residue passed through an alumina column, eluting with 2% methanol in methylene chloride to remove benzoic acid. The eluate was flash-chromatographed on silica gel, eluting with 5% methanol in methylene chloride, to yield 2.8 g of 2-(4-methylphenyl)-6-methylpyridine-N-oxide, m.p. 95° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05545645 |
| 出典データセット | uspto-grants-1996_08 |
| ORD ID | ord-6666939eed814061b84f82f13e26e1cd |
| 出典メモ | uspto-grants-1996_08 |