反应详情

温度

45 °C

11 mmol of silver carbonate and 20 mmol of 1-iodo-3-methoxypropane [61542-10-7] are added under an argon atmosphere to a solution of 21 mmol of 4-bromo-1H-pyridin-2-one [36953-37-4] in 30 ml of benzene. The reaction mixture is heated to 45° C. with exclusion of light for 2 days. The mixture is cooled to room temperature and filtered through Hyflo. The filtercake is washed with benzene and with saturated aqueous sodium hydrogencarbonate solution. The phases of the filtrate are separated and the aqueous phase is extracted with dichloromethane (3×). The combined organic phases are dried over sodium sulphate and concentrated by evaporation. The title compound is identified on the basis of the Rf value by means of flash chromatography (SiO2 60F).

1. temperatureThe mixture is cooled to room temperature
2. filtrationfiltered through Hyflo
3. washThe filtercake is washed with benzene and with saturated aqueous sodium hydrogencarbonate solution
4. customThe phases of the filtrate are separated
5. extractionthe aqueous phase is extracted with dichloromethane (3×)
6. dry with materialThe combined organic phases are dried over sodium sulphate
7. concentrationconcentrated by evaporation