反应详情

温度

60 °C

A mixture of intermediate 84 (0.39 g), DIEA (0.35 mL) and ethyl bromoacetate (0.22 mL) in acetonitrile was heated at 60° C. for 1.5 h. After evaporation of MeCN, the residue was extracted between EtOAc and saturated sodium bicarbonate. The organic phase was dried over sodium sulfate and evaporated to dryness. The crude product was purified by column chromatography with 70% to 90% EtOAc/Hex to give compound 83 (0.27 g, 57%). LCMS (+ESI) m/z=510.3 [M+H]+.

1. customAfter evaporation of MeCN
2. extractionthe residue was extracted between EtOAc and saturated sodium bicarbonate
3. dry with materialThe organic phase was dried over sodium sulfate
4. customevaporated to dryness
5. customThe crude product was purified by column chromatography with 70% to 90% EtOAc/Hex