反应详情

A mixture of 2-[4-(2-tert-butylphenyl)piperazin-1-yl]-2-oxoacetic acid (Example 44, 0.30 g, 1.03 mmol), methyl pyrrolidine-3-carboxylate hydrochloride (0.21 g, 1.2 mmol), triethylamine (215 μL, 1.6 mmol), EDCI (0.19 g, 1.2 mmol) and HOBt (0.19 g, 1.2 mmol) in N,N-dimethylformamide (5 mL) was stirred at room temperature for 2 days. The reaction mixture was poured into saturated NaHCO3 solution and extracted with ethyl acetate. The extract was washed with saturated NaHCO3 solution and brine, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate 85:15 to 35:65) to give the title compound (0.35 g, 85%) as a pale yellow oil.

1. extractionextracted with ethyl acetate
2. washThe extract was washed with saturated NaHCO3 solution and brine
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate 85:15 to 35:65)