反应详情

温度

120 °C

850 mg (2.2 mmol) of 2-(morpholin-4-ylmethyl)-7-[4-(trifluoromethyl)phenyl][1,2,4]triazolo-[1,5-c]pyrimidin-5-ol (Example 135A) are introduced into phosphoryl chloride (20 ml), 1.98 g (8.7 mmol) of benzyltriethylammonium chloride are added, and the reaction mixture is stirred at 120° C. for 2 h. The reaction mixture is slowly poured, while stirring vigorously, into ice-water, and solid sodium bicarbonate is added until a pH of 8 is reached. The reaction mixture is extracted with ethyl acetate (150 ml), and the organic phase is separated off, dried (magnesium sulphate) and concentrated. The residue is chromatographed on silica gel (mobile phase dichloromethane/ethanol 100:1 to 20:1). 650 mg (75% of theory) of the product are obtained as a solid.

1. additionare added
2. additionThe reaction mixture is slowly poured
3. additionis added until a pH of 8
4. extractionThe reaction mixture is extracted with ethyl acetate (150 ml)
5. customthe organic phase is separated off
6. dry with materialdried (magnesium sulphate)
7. concentrationconcentrated
8. customThe residue is chromatographed on silica gel (mobile phase dichloromethane/ethanol 100:1 to 20:1)
9. custom650 mg (75% of theory) of the product are obtained as a solid