反应详情

温度

160 °C

A mixture of 6-chloro-9-vinylpurine (0.18 g, 1 mmol), 4-dimethylphosphinylaniline (0.17 g, 1 mmol), and pyridine hydrochloride (0.11 g, 1 mmol) was dissolved in 2-ethoxyethanol (2 mL). The resulting solution was heated at 160° C. for 10 minutes under microwave irradiation. The mixture was concentrated to dryness on a rotavap. EtOAc and aq. NaHCO3 were added. The aqueous layer was extracted with ethyl acetate and the combined organic layers were dried over sodium sulfate, concentrated on a rotavap, and then subjected to silica gel column chromatography (eluent: 10% methanol/methylene chloride) yielding the desired product.

1. concentrationThe mixture was concentrated to dryness on a rotavap
2. additionEtOAc and aq. NaHCO3 were added
3. extractionThe aqueous layer was extracted with ethyl acetate
4. dry with materialthe combined organic layers were dried over sodium sulfate
5. concentrationconcentrated on a rotavap