反应详情

A suspension of 1-(2-tert-butylphenyl)piperazine dihydrochloride (Reference Example 1, 0.400 g, 1.37 mmol), (2,5-dioxoimidazolidin-4-yl)acetic acid (0.261 g, 1.65 mmol), EDCI (0.311 g, 1.65 mmol), HOBt (0.223 g, 1.65 mmol) and triethylamine (496 μl, 3.56 mmol) in DMF (13 mL) was stirred at room temperature for 16 h. The reaction mixture was poured into saturated ammonium chloride solution and extracted with ethyl acetate. The organic layer was washed with saturated sodium hydrogen carbonate solution and brine, dried over MgSO4, and the solvent was evaporated under reduced pressure to give crude product. The product was purified by re-crystallization from THF and n-hexane to provide 5-{2-[4-(2-tert-butylphenyl)piperazin-1-yl]-2-oxoethyl}imidazolidine-2,4-dione (0.344 g, 70%) as a white powder.

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with saturated sodium hydrogen carbonate solution and brine
3. dry with materialdried over MgSO4
4. customthe solvent was evaporated under reduced pressure
5. customto give crude product
6. customThe product was purified by re-crystallization from THF and n-hexane