反应详情

温度

0 °C

To a solution of compound 1b (6.00 g, 33.3 mmol) in DMF (100 mL) was added ethyl 3-bromo-2-oxopropanoate (8.00 g, 41.0 mmol) dropwise with stirring. The resulting solution was stirred at rt overnight. The reaction mixture was cooled to 0° C. The solids were collected by filtration and washed with Et2O (3×100 mL). Compound 1c was obtained as a white solid (8.40 g, 81% yield). Mass Spectrum (LCMS, ESI pos.): Calcd. for C13H16N4O3: 276.1 (M+H). found: 276.3.

1. stirringThe resulting solution was stirred at rt overnight
2. filtrationThe solids were collected by filtration
3. washwashed with Et2O (3×100 mL)