反应详情

A solution of N-methylpropionohydrazide (18.78 g, 183.9 mmol) and diethyl ketomalonate (56.1 mL, 368 mmol) in toluene (136 mL) was refluxed with a Dean-Stark trap for 4 hours. The reaction mixture was concentrated under reduced pressure to give the crude material that was purified by silica gel flash column chromatography (100% hexanes to 5 to 10% EtOAc in hexanes) to afford 23 g (49%) of the desired product.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. customto give the crude material that
3. customwas purified by silica gel flash column chromatography (100% hexanes to 5 to 10% EtOAc in hexanes)