反应详情

2,5-Difluoro-nitrobenzene (21.5 g), 1-benzyl-4-amino-piperidine (52.3 g) and N-methyl-piperidone (100 ml) were stirred at 100° C. for 3 h. After cooling the mixture was partitioned between water and ethyl acetate and the aqueous layer was extracted twice with ethyl acetate. The combined organic layers were extracted 5 times with water, and the solvent was evaporated in vacuo. The target compound was crystallized from methanol to yield 38.7 g of the title compound as orange crystals (mp. 86-87° C.).

1. temperatureAfter cooling the mixture
2. customwas partitioned between water and ethyl acetate
3. extractionthe aqueous layer was extracted twice with ethyl acetate
4. extractionThe combined organic layers were extracted 5 times with water
5. customthe solvent was evaporated in vacuo
6. customThe target compound was crystallized from methanol