反应详情

温度

45 °C

A mixture of 113.26 mmol of 5-bromo-3-(3-methoxypropoxy)-1H-pyridin-2-one, 79.28 mmol of silver carbonate and 158.56 mmol of iodomethane in 230 ml of benzene is stirred at 45° C. with exclusion of light for 24 hours. The reaction mixture is cooled to room temperature, and the silver salts are filtered off. The filtrate is washed with 2% sodium bicarbonate solution and water (2×). The organic phase is dried over sodium sulphate and evaporated. The crude title compound is obtained as a beige oil from the residue and is employed without further purification in the next stage. Rf=0.45 (EtOAc-heptane 1:2); Rt=4.34 (Gradient I).

1. temperatureThe reaction mixture is cooled to room temperature
2. filtrationthe silver salts are filtered off
3. washThe filtrate is washed with 2% sodium bicarbonate solution and water (2×)
4. dry with materialThe organic phase is dried over sodium sulphate
5. customevaporated