反应详情

To a solution of L-alanine ethyl ester hydrochloride (50 g, 325 mmol) in anhydrous dichloromethane (800 mL) added triethylamine (65.8 g, 650 mmol) and stirred at room temperature for 30 minutes. To the reaction mixture cyclopropanecarbonyl chloride (50.96 g, 0.487 mole) was slowly added and stirred at room temperature for overnight. The reaction mixture was then poured into a cold solution of saturated aqueous sodium bicarbonate, and the crude product extracted with dichloromethane, dried over anhydrous magnesium sulfate. Evaporation of the solvent gave a crude residue, which was purified by column chromatography on silica gel using a mixture of ethyl acetate:hexane (1:1) as eluant to give 2-(cyclopropanecarbonyl-amino)-propionic acid ethyl ester (163) (58.0 g, 96% yield).

1. stirringstirred at room temperature for overnight
2. extractionthe crude product extracted with dichloromethane
3. dry with materialdried over anhydrous magnesium sulfate
4. customEvaporation of the solvent
5. customgave a crude residue, which
6. customwas purified by column chromatography on silica gel using
7. additiona mixture of ethyl acetate:hexane (1:1) as eluant