関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus tribromide | HCID 24614 | — |
| 反応物 | (6-Chloro-2-methylpyridin-3-yl)methanol | HCID 59525984 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-(Bromomethyl)-6-chloro-2-methylpyridine | HCID 59526174 | — |
反応手順
(6-Chloro-2-methylpyridin-3-yl)methanol (500 mg, 3.17 mmol) was taken up in dichloromethane (9.1 mL) and cooled to 0° C. Phosphorus tribromide (0.6 mL, 6.35 mmol) was added dropwise, and the reaction was allowed to warm to room temperature overnight. The reaction was then quenched by slow addition of saturated aqueous sodium bicarbonate, followed by solid sodium carbonate to obtain pH>7. The mixture was extracted with dichloromethane two times. The combined organic layers were dried over magnesium sulfate, filtered, and concentrated under reduced pressure. Purification was performed via silica gel chromatography (0-40% ethyl acetate in hexane) to yield the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08367706B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-b4df6cbfdea64a09926bf2aace03af63 |
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| 出典メモ | uspto-grants-2013_02 |
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