関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,3-Lutidine | HCID 11420 | — |
| 反応物 | Sodium Sulfite | HCID 24437 | — |
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Pyridine, 2,3-dimethyl-, 1-oxide | HCID 3840573 | 50.1% |
反応手順
In methylene chloride (200 ml) was dissolved 2,3-dimethylpyridine (9.50 g) and the resulting solution was. cooled to 0° C. Metachloroperbenzoic acid (21.9 g) was added to the reaction mixture, followed by heating to room temperature. Stirring was conducted for 3 days. An aqueous solution of sodium sulfite was added and the resulting mixture was separated using methylene chloride (200 ml). The organic layer was dried over anhydrous magnesium sulfate, the filtrate was concentrated and the concentrate was purified by chromatography on a silica gel column (5% methanol—methylene chloride). Petroleum ether was added to the residue. Colorless powder so precipitated was collected by filtration, followed by drying, whereby the title compound (5.47 g) was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06747023B1 |
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| 出典データセット | uspto-grants-2004_06 |
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| ORD ID | ord-68e958ca661d45c6ae2ebf8889725afc |
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| 出典メモ | uspto-grants-2004_06 |
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