反应详情

A solution of ethyl 3-[4-(3-nitrophenyl)piperazino]propanoate D6 (3.00 g, 9.76 mmol) and hydrazine monohydrate (2.93 g, 2.85 mL, 58.56 mmol) in ethanol (30 mL) was refluxed for 24 hrs. The solvent was evaporated under reduced pressure, brine was added to the residue and the product was extracted several times with dichloromethane. The combined organic phases were dried over MgSO4 and the solvent was evaporated under reduced pressure to afford 3.00 g crude product as an orange semi-solid. Purification by flash chromatography (Silica gel 60 Å, 45 μm, 10% methanol in dichloromethane) afforded 0.55 g (19%) 3-[4-(3-nitrophenyl)piperazino]propanohydrazide D7.

1. customThe solvent was evaporated under reduced pressure, brine
2. additionwas added to the residue
3. extractionthe product was extracted several times with dichloromethane
4. dry with materialThe combined organic phases were dried over MgSO4
5. customthe solvent was evaporated under reduced pressure
6. customto afford 3.00 g crude product as an orange semi-solid
7. customPurification by flash chromatography (Silica gel 60 Å, 45 μm, 10% methanol in dichloromethane)