反应详情

To a suspension of sodium acetate (30.76 g, 375 mmol) in DMF (250 mL) was added dropwise tert-Butyl 2-bromo-acetoacetate (59.27 g, 250 mmol). After stirring at ambient temperature for 90 minutes, water (415 mL) was added, followed by extraction with ethyl acetate (3×325 mL). The combined organic layers were washed with water (3×325 mL) and brine (325 mL), dried over Na2SO4 and after filtration, the solvent was removed in vacuo. The resulting oil was purified by distillation (12 mbar, 128°)

1. extractionfollowed by extraction with ethyl acetate (3×325 mL)
2. washThe combined organic layers were washed with water (3×325 mL) and brine (325 mL)
3. dry with materialdried over Na2SO4
4. filtrationafter filtration
5. customthe solvent was removed in vacuo
6. distillationThe resulting oil was purified by distillation (12 mbar, 128°)