反应详情

To a suspension of diethyl 2-aminomalonate hydrochloride (4.2 g) in tetrahydrofuran are added triethylamine (2.1 g) and N-(chloroacetyl)glycine (3.0 g), and the mixture is cooled to 0° to 5° C. To the mixture is further added N,N'-dicyclohexylcarbodiimide (4.3 g), and the mixture is stirred at the same temperature for 2 hours and then allowed to stand at room temperature overnight. Insoluble substance is filtered off from the reaction mixture, and the filtrate is concentrated under reduced pressure. To the residue is added ethyl acetate, and the insoluble substance is filtered off. The filtrate is concentrated under reduced pressure, and the residue is recrystallized from ethyl acetateisopropyl ether to give diethyl 2-[[N-(chloroacetyl)glycyl]amino]malonate (5.1 g), m.p. 104.5°-105° C.

1. temperaturethe mixture is cooled to 0° to 5° C
2. waitto stand at room temperature overnight
3. filtrationInsoluble substance is filtered off from the reaction mixture
4. concentrationthe filtrate is concentrated under reduced pressure
5. additionTo the residue is added ethyl acetate
6. filtrationthe insoluble substance is filtered off
7. concentrationThe filtrate is concentrated under reduced pressure
8. customthe residue is recrystallized from ethyl acetateisopropyl ether