反应详情

温度

0 °C

An ice cold solution of 2-oxo-1-pyrrolidineacetic acid (1.03 g) and triethylamine (1.01 ml) in dichloromethane (20 ml) was treated dropwise with butyl chloroformate (0.92 ml). After stirring at 0° C. for 30 minutes a suspension of 1-(2-aminoacetyl)-2,2-dimethyl-4-imidazolidinone hydrobromide (1.82 g) and triethylamine (1.01 ml) in dichloromethane (20 ml) was added, and the temperature was gradually raised to room temperature. After stirring at room temperature for 1 day the suspension was evaporated under reduced pressure. The residue was chromatographed on a silica/gel column eluting with methanol/dichloromethane 1:1. The selected fractions were collected and evaporated, the residue was washed with ethyl acetate and crystallized from ethanol to give the title compound as a white solid, m.p. 229°-231° C.

1. additionwas added
2. temperaturethe temperature was gradually raised to room temperature
3. stirringAfter stirring at room temperature for 1 day the suspension
4. customwas evaporated under reduced pressure
5. customThe residue was chromatographed on a silica/gel column
6. washeluting with methanol/dichloromethane 1:1
7. customThe selected fractions were collected
8. customevaporated
9. washthe residue was washed with ethyl acetate
10. customcrystallized from ethanol