反应详情

温度

65 °C

Into a 50 mL sealed tube, was placed a solution of compound 90f (3.50 g, 8.53 mmol) in ethylene glycol dimethyl ether (35 mL). To the stirring mixture, ethyl 3-bromo-2-oxopropanoate (5.25 g, 26.9 mmol) was added drop-wise at 0° C. The reaction mixture was stirred overnight at 65° C. and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel (EtOAc/petroleum ether (3:1 v/v)) to obtain compound 90g as a yellow solid (560 mg, 13% yield). Mass Spectrum (LCMS, ESI pos.): Calcd. for C23H29ClN6O4: 487.0 (M+H). found 487.1.

1. customInto a 50 mL sealed tube
2. concentrationconcentrated under reduced pressure
3. customThe residue was purified by flash column chromatography on silica gel (EtOAc/petroleum ether (3:1 v/v))