反应详情

温度

50 °C

In 300 ml of phosphorus oxychloride was added dropwise 28 ml of N,N-dimethylaniline, and 30.5 g of 2,5-bis(acetoxymethyl)-7-hydroxy-s-triazolo[1,5-a]pyrimidine was added to the mixture and the mixture was stirred at 50 ° C. for 1.5 hours. An oily residue obtained by removing phosphorus oxychloride was dissolved in 500 ml of chloroform and ice-cooled. After addition of crushed ice and water to the mixture and stirring thereof, a chloroform layer was separated, washed with water and dried over anhydrous magnesium sulfate. Then, the mixture was condensed. This was applied to a silica gel column chromatography (eluent chloroform) and fractions containing the title compound were condensed to obtain 14 g of the title compound as an oily product.

1. additionwas added to the mixture
2. customAn oily residue obtained
3. customby removing phosphorus oxychloride
4. dissolutionwas dissolved in 500 ml of chloroform
5. temperatureice-cooled
6. additionAfter addition of crushed ice and water to the mixture
7. stirringstirring
8. customa chloroform layer was separated
9. washwashed with water
10. dry with materialdried over anhydrous magnesium sulfate
11. customcondensed