反应详情

温度

0 °C

An ice cold solution of 2-oxo-1-pyrrolidineacetic acid (1.45 g) and triethylamine (1.45 ml) in dimethylformamide (7 ml) was treated dropwise while stirring with butyl chloroformate (1.3 ml). After stirring at 0° C. for 45 minutes, 2,2-dimethyl-5-oxo-1-imidazolidineacetamide (1.75 g) was added at once and stirring was prolonged at room temperature overnight. After evaporation under reduced pressure, the residue was chromatographed on a silica gel column, eluting with dichloromethane/methanol 1:1. The selected fractions were collected and evaporated, the residue was taken up with ethyl acetate and the resulting solid was crystallized from ethanol, to give the title compound as a white powder, m.p. 225°-227° C., (decomp.).

1. stirringstirring
2. waitwas prolonged at room temperature overnight
3. customAfter evaporation under reduced pressure
4. customthe residue was chromatographed on a silica gel column
5. washeluting with dichloromethane/methanol 1:1
6. customThe selected fractions were collected
7. customevaporated
8. customthe resulting solid was crystallized from ethanol