반응 #44242

반응 방정식

N-methylpropionohydrazide

diethyl ketomalonate

→

desired product

수율 49.0%

diethyl 2-(2-methyl-2-propionylhydrazono)malonate

수율 49.0%

용매

toluene

반응 조건

후처리

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

실험 절차

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.

출처