反应详情

温度

80 °C

To a solution of 4-(2-bromo-5-fluorophenoxy)-1-[5-(1H-pyrrol-3-yl)-1,2,4-oxadiazol-3-yl]piperidine (60 mg, 0.15 mmol) in DMF (491 μL) was added sodium hydride (11.8 mg, 0.3 mmol). After 5 min, ethyl bromoacetate (25 μL, 0.22 mmol) was added and the mixture was heated at 80° C. for 3 h. The mixture was poured onto ice cold 1N HCl (2 mL) and extracted with EtOAc (3×2 mL). The combined organic fractions were washed with water (2 mL) and then dried over Na2SO4. The solvent was evaporated. Purification by Combiflash chromatography (SiO2-12 g, gradient elution of 30-60% EtOAc/hexanes over 25 min) gave the title compound.

1. additionThe mixture was poured onto ice cold 1N HCl (2 mL)
2. extractionextracted with EtOAc (3×2 mL)
3. washThe combined organic fractions were washed with water (2 mL)
4. dry with materialdried over Na2SO4
5. customThe solvent was evaporated
6. customPurification
7. washby Combiflash chromatography (SiO2-12 g, gradient elution of 30-60% EtOAc/hexanes over 25 min)