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HRID 588370作成日:2026年10月26日

Water → 2-Chloro-3-methyl-1-oxo-1lambda~5~-pyridine

https://huagongshe.com/reaction/588370

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物Trifluoroacetic anhydrideHCID 9845—
反応物Carbamide PeroxideHCID 31294—
反応物2-Chloro-3-methylpyridineHCID 87603—
溶媒DichloromethaneHCID 6344—
生成物2-Chloro-3-methyl-1-oxo-1lambda~5~-pyridineHCID 1343162286%

反応手順

To a mixture of 2-chloro-3-methylpyridine (15 g, 118 mmol) and urea hydrogen peroxide (44.07 g, 468.5 mmol) in DCM (300 mL) was added trifluoroacetic anhydride (98.55 g, 469.2 mmol) dropwise at 0° C. The mixture was stirred at room temperature for 20 h. The mixture was then poured into water (150 mL), and the layers were separated. The organic layer was washed with saturated aqueous Na2S2O3 (20 mL), dried over Na2SO4, filtered, and the filtrate was concentrated under reduced pressure. The crude product was purified by silica gel flash chromatography (DCM:MeOH, 100:0 to 10:1) to afford the title compound (14.5 g, 86%) as a colorless solid.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09227956B2
出典データセットuspto-grants-2016_01
ORD IDord-9b19f3851e914078a67b2c5d960f976f
出典メモuspto-grants-2016_01