反应详情

温度

120 °C

950 mg (2.7 mmol) of 7-(2,4-dichlorophenyl)-2-(trifluoromethyl)[1,2,4]triazolo[1,5-c]pyrimidin-5-ol (Example 130A) are introduced into phosphoryl chloride (10 ml), 1.86 g (8.2 mmol) of benzyltriethylammonium chloride are added, and the reaction mixture is stirred at 120° C. for 12 h. The reaction mixture is slowly poured, with vigorous stirring, into saturated sodium bicarbonate solution and ice, and solid sodium bicarbonate (approx. 5 g) is added until a pH of 8 is reached. The solid is filtered off with suction. The reaction vessel is washed out with dichloromethane, and the organic phase is dried over magnesium sulphate, concentrated and combined with the filtered solid. The crude product is purified by silica gel chromatography (cyclohexane/ethyl acetate 10:1). 784 mg (78% of theory) of the product are obtained.

1. additionare added
2. additionis added until a pH of 8
3. filtrationThe solid is filtered off with suction
4. washThe reaction vessel is washed out with dichloromethane
5. dry with materialthe organic phase is dried over magnesium sulphate
6. concentrationconcentrated
7. customThe crude product is purified by silica gel chromatography (cyclohexane/ethyl acetate 10:1)
8. custom784 mg (78% of theory) of the product are obtained