反应详情

温度

40 °C

To a suspension of milled potassium carbonate (38.7 g, 0.28 mol) in DMSO (100 mL) was added (3,4-dichlorophenyl)methyl azide (Intermediate 3) (14 g, 0.07 mol) and methyl acetoacetate (12.1 g, 0.1 mol). The mixture was stirred at 40° C. for 48 hours. The mixture was poured into a mixture of ice and water (100 mL). The water was extracted with ethyl acetate (100 mL×2). The combined organic phases were dried over sodium sulfate, filtered and concentrated. The residue was purified by distillation to give the title compound as white solid crystals (14 g, 67%). LC/MS: m/z 301 (M+H)+, Rt: 1.97 min.

1. extractionThe water was extracted with ethyl acetate (100 mL×2)
2. dry with materialThe combined organic phases were dried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated
5. distillationThe residue was purified by distillation