反应详情

Diethyl 2-aminomalonate hydrochloride (4.2 g), formylglycine (2.3 g) and 1-hydroxybenzotriazole (2.7 g) are dissolved in dimethylformamide (50 ml). To the solution are added N,N'-dicyclohexylcarbodiimide (4.33 g) and triethylamine (2.12 g) at 0° to 5° C. The mixture is stirred at the same temperature for 2 hours and at room temperature for 15 hours. The reaction mixture is concentrated under reduced pressure. To the residue is added ethyl acetate, and the mixture is filtered to remove insoluble materials. The filtrate is washed, dried and evaporated to remove the solvent. The residue is purified by silica gel column chromatography [solvent; chloroform-ethyl acetate (1:5)]to give diethyl 2-[(N-formylglycyl)amino]malonate (4.1 g), m.p. 95°-96° C.

1. concentrationThe reaction mixture is concentrated under reduced pressure
2. additionTo the residue is added ethyl acetate
3. filtrationthe mixture is filtered
4. customto remove insoluble materials
5. washThe filtrate is washed
6. customdried
7. customevaporated
8. customto remove the solvent
9. customThe residue is purified by silica gel column chromatography [solvent