反应详情

700 mg (2.9 mmol) of 5,7-dimethyl-2-phenylimidazo[5,1-f][1,2,4]triazin-4(3H)-one (Example 15A) were dissolved in 8 ml of phosphoryl chloride and stirred at reflux for 12 h. The reaction mixture was poured into 170 ml of saturated sodium bicarbonate solution, and solid sodium bicarbonate was added until a pH of 7 had been reached. Ethyl acetate was added, and the mixture was extracted. The organic phase was washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate and concentrated on a rotary evaporator. This gave 657 mg (80% of theory) of the product as a solid.

1. temperatureat reflux for 12 h
2. additionwas added until a pH of 7
3. extractionthe mixture was extracted
4. washThe organic phase was washed with saturated aqueous sodium chloride solution
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated on a rotary evaporator