反应详情

温度

65 °C

A solution of 34C (72 mg, 0.27 mmol) in DMF (4 mL) was treated with 4-(methoxycarbonyl)benzoic acid (78 mg, 0.43 mmol), HOBt (66 mg, 0.43 mmol) and triethylamine (100 mg, 1.0 mmol). The solution was treated with EDCI (96 mg, 0.5 mmol) at room temperature for 15 minutes, and then warmed to 65° C. for 16 hours. The reaction mixture was partitioned between EtOAc (20 mL) and 1 M HCl (20 mL). The organic layer was washed with 1 N HCl (20 mL), 1 N NaOH (20 mL) and brine (20 mL). The reaction was dried (Na2SO4), filtered, and concentrated to a solid. The crude material was purified by chromatography (SiO2, 1:2 EtOAc in heptane) to afford 34D (99 mg, 85%).

1. customThe reaction mixture was partitioned between EtOAc (20 mL) and 1 M HCl (20 mL)
2. washThe organic layer was washed with 1 N HCl (20 mL), 1 N NaOH (20 mL) and brine (20 mL)
3. dry with materialThe reaction was dried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated to a solid
6. customThe crude material was purified by chromatography (SiO2, 1:2 EtOAc in heptane)