反应详情

To a solution of n-Boc-piperazine (1.08 g, 5.80 mmol) in dry DMF (10 mL) were added anhydrous potassium carbonate (4.01 g, 29.04 mmol) and compound 26 (1.5 g, 6.97 mmol). The reaction mixture was stirred at RT for 8 h. The potassium carbonate was removed by suction filtration and the solvent was removed under reduced pressure. The residue was dissolved with water and extracted with ethyl acetate. The combined organic layers were dried over anhydrous sodium sulfate and the solvent was removed by evaporation. The crude product was purified by column chromatography using ethyl acetate:hexane (8:2) to give compound 28 (1.58 g, 85%). 1H NMR (400 MHz, CDCl3) δ 1.39 (s, 9H), 1.92 (s, 2H), 2.36 (s, 4H), 2.48 (s, 2H), 3.39 (s, 4), 3.95 (m, 2), 6.83 (m, 2H), 7.19 (m, 3H).

1. customThe potassium carbonate was removed by suction filtration
2. customthe solvent was removed under reduced pressure
3. dissolutionThe residue was dissolved with water
4. extractionextracted with ethyl acetate
5. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
6. customthe solvent was removed by evaporation
7. customThe crude product was purified by column chromatography