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HRID 1033113作成日:2026年10月25日

Chloromethyl Methyl Ether → Diethyl 1-(methoxymethyl)-2,5-dioxo-4-imidazolylphosphonate

https://huagongshe.com/reaction/1033113

反応式

関与物質

役割名称HCID仕込み量
反応物Chloromethyl Methyl EtherHCID 7864—
反応物Sodium hydrideHCID 24758—
反応物Diethyl (2,5-dioxo-2,5-dihydro-1H-imidazol-4-yl)phosphonateHCID 53733419—
溶媒Diethyl EtherHCID 3283—
溶媒DimethylformamideHCID 6228—
溶媒Ethyl AcetateHCID 8857—
生成物Diethyl 1-(methoxymethyl)-2,5-dioxo-4-imidazolylphosphonateHCID 53791991—

反応手順

To a solution of diethyl 2,5-dioxo-4-imidazolylphosphonate (3.61 g, 0.015 moles) in DMF (10 mL), under N2, is added sodium hydride (80% dispersion in oil) (0.55 g, 0.018 moles) and stirred for 5 minutes. Chloromethyl methyl ether (tech. grade 85%) (1.9 mL, 0.021 moles) is added. This mixture is stirred at room temperature for 4 hours, diluted with ether and ethyl acetate (300 mL) and then washed with water and brine before drying over MgSO4. The aqueous layer is back extracted with methylene chloride and combined with the previous organic fraction. Evaporation of solvents and chromatography (eluant 1% methanol in chloroform) and evaporation under high vacuum affords the required product.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05308853
出典データセットuspto-grants-1994_05
ORD IDord-b827a0970433490393d7126541b0b1b2
出典メモuspto-grants-1994_05