反应详情

温度

120 °C

927 mg (4.19 mmol) of 7-chloro[1,2,4]triazolo[1,5-c]pyrimidin-5-ol (Example 52A) are suspended in 16.9 g (110.13 mmol) of phosphoryl chloride under argon and heated at 120° C. for 4 h. After this time, the excess phosphoryl chloride is removed in vacuo, and the residue is distilled together with toluene. The residue is suspended in water, the pH is brought to 7 with saturated aqueous sodium bicarbonate solution, and the precipitated solid is filtered off with suction. The latter is washed with water and dried over phosphorus pentoxide for 18 h. 389 mg (49% of theory) of the product are obtained.

1. customAfter this time, the excess phosphoryl chloride is removed in vacuo
2. distillationthe residue is distilled together with toluene
3. filtrationthe precipitated solid is filtered off with suction
4. washThe latter is washed with water
5. dry with materialdried over phosphorus pentoxide for 18 h
6. custom389 mg (49% of theory) of the product are obtained