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HRID 64492作成日:2026年10月25日

Citric Acid → Diethyl butyl[({8-[(2,6-difluorobenzyl)oxy]-2-methylimidazo[1,2-a]pyridin-3-yl}carbonyl)amino]malonate

https://huagongshe.com/reaction/64492

反応式

関与物質

役割名称HCID仕込み量
反応物Citric AcidHCID 311—
反応物Butyl iodideHCID 10962—
反応物Sodium BicarbonateHCID 516892—
反応物Sodium ethoxideHCID 2723922—
反応物Ethanol sodium ethoxideHCID 23706232—
反応物Diethyl[({8-[(2,6-difluorobenzyl)oxy]-2-methylimidazo[1,2-a]pyridin-3-yl}carbonyl)amino]malonateHCID 86713528—
溶媒EthanolHCID 702—
溶媒ChloroformHCID 6212—
生成物Diethyl butyl[({8-[(2,6-difluorobenzyl)oxy]-2-methylimidazo[1,2-a]pyridin-3-yl}carbonyl)amino]malonateHCID 86713527—

反応条件

温度70 °C

反応手順

To 252 mg of diethyl[({8-[(2,6-difluorobenzyl)oxy]-2-methylimidazo[1,2-a]pyridin-3-yl}carbonyl)amino]malonate were added 4 ml of ethanol, 0.23 ml of a 20% sodium ethoxide/ethanol solution, and 0.31 ml of 1-iodobutane, followed by stirring at 70° C. for 3 hours. Subsequently, 11 mg of sodium ethoxide was added thereto, followed by stirring at 70° C. for 1 hour. To the reaction mixture were added an aqueous citric acid solution, a saturated aqueous sodium hydrogen carbonate solution, and chloroform to carry out a layer separation operation. The organic layer was dried over anhydrous sodium sulfate and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain 69 mg of diethyl butyl[({8-[(2,6-difluorobenzyl)oxy]-2-methylimidazo[1,2-a]pyridin-3-yl}carbonyl)amino]malonate.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09447090B2
出典データセットuspto-grants-2016_09
ORD IDord-af7d2113700a453d8a8cb158194c14ec
出典メモuspto-grants-2016_09