関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | 3-Bromo-2-chloro-6-methylpyridine | HCID 2734418 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 3-Bromo-2-chloro-6-methylpyridin-1-ium-1-olate | HCID 85706489 | 1,230.1% |
反応手順
step a—To a solution of 3-bromo-2-chloro-6-methyl-pyridine (2.0 g, 0.687 mmol) in CHCl3 was added MCPBA (3.3 g, 19.1 mmol) and the resulting solution was heated at 50° C. overnight. The resulted solution was cooled and partitioned between DCM and sat'd. aq. NaHCO3. The organic layer was dried (Na2SO4), filtered and concentrated in vacuo. The crude product was purified by SiO2 chromatography eluting with an EtOAc/hexane gradient (30 to 80% EtOAc) to afford 1.88 g (87%) of 3-bromo-2-chloro-6-methyl-pyridine 1-oxide (357a) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08273773B2 |
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| 出典データセット | uspto-grants-2012_09 |
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| ORD ID | ord-018b7ca9aaaf4f3b845ebada39f7db3d |
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| 出典メモ | uspto-grants-2012_09 |
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