反应详情

温度

120 °C

530 mg (1.30 mmol) of 7-(2,4-dichlorophenyl)-2-[1-(1-methylethyl)piperidin-4-yl][1,2,4]-triazolo[1,5-c]pyrimidin-5(6H)-one were initially charged in phosphorus oxychloride (16 ml), and 1.19 g (5.22 mmol) of benzyltriethylammonium chloride were added. The mixture was then stirred at 120° C. for 2.5 h. The reaction mixture was poured onto saturated aqueous sodium bicarbonate solution (150 ml), and solid sodium bicarbonate was added until a pH of 7 had been reached. The mixture was extracted with dichloromethane (3×50 ml), and the combined organic phases were washed with water (50 ml), dried over magnesium sulfate and concentrated. This gave 502 mg (89% of theory) of the product as a solid.

1. additionwas added until a pH of 7
2. extractionThe mixture was extracted with dichloromethane (3×50 ml)
3. washthe combined organic phases were washed with water (50 ml)
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated