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HRID 1847015作成日:2026年10月26日

Sodium hydride → 5-[2-(1,3-Dioxolan-2-yl)ethyl]-3-methoxypyrido[2,3-b]pyrazin-6 (5H)-one

https://huagongshe.com/reaction/1847015

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium hydrideHCID 24758—
反応物Lithium BromideHCID 82050—
反応物2-(2-Bromoethyl)-1,3-dioxolaneHCID 87776—
反応物3-Methoxypyrido[2,3-b]pyrazin-6(5H)-oneHCID 57815366—
溶媒WaterHCID 962—
溶媒DimethylformamideHCID 6228—
生成物5-[2-(1,3-Dioxolan-2-yl)ethyl]-3-methoxypyrido[2,3-b]pyrazin-6 (5H)-oneHCID 86724945—

反応手順

3-Methoxypyrido[2,3-b]pyrazin-6(5H)-one (400 mg, 2.26 mmol) was dissolved in N,N-dimethylformamide (12 ml). Lithium bromide (206 mg, 2.37 mmol) and sodium hydride (55%, 104 mg, 2.37 mmol) were added to the solution under cooling on ice and stirred for one and a half hours while the temperature of the reaction solution was raised to room temperature. The reaction solution was cooled on ice again, 2-(2-bromoethyl)-1,3-dioxolane (0.345 mmol, 2.94 mmol) was added thereto and the mixture was stirred at room temperature for 22 hours. Water was added to the reaction solution, which was then extracted with ethyl acetate and washed with saturated sodium chloride solution. After drying over anhydrous sodium sulfate, the solvent was removed under reduced pressure. The residue was purified by silica gel column chromatography (chloroform/methanol) to yield 731 mg (quantitative) of the title compound in the form of a yellow oily product.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08952010B2
出典データセットuspto-grants-2015_02
ORD IDord-26d43389f48840b1a74a3c4a2c19934a
出典メモuspto-grants-2015_02