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HRID 385946作成日:2026年10月25日

Phosphorus tribromide → 3-(Bromomethyl)-6-chloro-2-methylpyridine

https://huagongshe.com/reaction/385946

反応式

関与物質

役割名称HCID仕込み量
反応物Phosphorus tribromideHCID 24614—
反応物(6-Chloro-2-methylpyridin-3-yl)methanolHCID 59525984—
溶媒DichloromethaneHCID 6344—
生成物3-(Bromomethyl)-6-chloro-2-methylpyridineHCID 59526174—

反応条件

温度0 °C

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US08367706B2
出典データセットuspto-grants-2013_02
ORD IDord-b4df6cbfdea64a09926bf2aace03af63
出典メモuspto-grants-2013_02