反应详情

To a solution of 7-ethoxy-7-oxoheptanoic acid (2.0 g, 10.6 mmol) in DMF (50 mL) were added HBTU (4.4 g, 11.6 mmol), DIEA (4.1 g, 31.8 mmol) at room temperature. The resulting mixture was stirred for 10 min, then tert-butyl (2-aminophenyl)carbamate (2.43 g, 11.7 mmol) was added to the reaction solution. The reaction mixture was stirred for 12 h at room temperature. The reaction was quenched with water (200 mL). The resulting mixture was extracted by EtOAc (200 mL×2). The organic layers were combined, dried with anhydrous Na2SO4 and concentrated under reduced pressure. The resulting solid was purified by column chromatography (elute: EtOAc:PE (petroleum ether)=1:4) to afford the desired compound (3.7 g, yield 92.1%) as a light yellow oil.

1. stirringThe reaction mixture was stirred for 12 h at room temperature
2. customThe reaction was quenched with water (200 mL)
3. extractionThe resulting mixture was extracted by EtOAc (200 mL×2)
4. dry with materialdried with anhydrous Na2SO4
5. concentrationconcentrated under reduced pressure
6. customThe resulting solid was purified by column chromatography (elute: EtOAc:PE (petroleum ether)=1:4)