反应详情

温度

25 °C

A mixture of 2-carboxymethyl-2-(pyrrol-1-yl)-malonic acid diethyl ester (36.0 g), N-hydroxysuccinimide (16.1 g) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (29.2 g) in dichloromethane (200 ml) was stirred at 25° C. for 1 hour, followed by addition of 7.8% (w/w) ammonia in acetonitrile (110 ml). The resulting mixture was stirred at 25° C. for 1 hour and concentrated under reduced pressure at the same temperature. The residue was dissolved in ethyl acetate. The solution was washed with 5% hydrochloric acid and then with saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and evaporated under reduced pressure. The residue was recrystallized from ethyl acetate/n-hexane to give the title compound (29.0 g, 80.8%) as colorless crystals, mp 94°-95° C.

1. stirringThe resulting mixture was stirred at 25° C. for 1 hour
2. concentrationconcentrated under reduced pressure at the same temperature
3. dissolutionThe residue was dissolved in ethyl acetate
4. washThe solution was washed with 5% hydrochloric acid
5. dry with materialwith saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate
6. customevaporated under reduced pressure
7. customThe residue was recrystallized from ethyl acetate/n-hexane