反应详情

To an ice-cooled mixture of 30.5 g (0.15 mole) of 7-hydroxy-5-methoxycarbonyl-2-methyl-s-triazolo[1,5-a]pyrimidine and 300 ml of phosphorus oxychloride, 18.6 ml (0.15 ml) of N,N-dimethylaniline was added dropwise over 5 minutes and the mixture was stirred under reflux for 1 hour, followed by concentration. The residue obtained was dissolved in 300 ml of chloroform and washed with water, followed by drying over anhydrous magnesium sulfate. The solvent was evaporated and n-hexane was added to the set residue. The crystals were collected by filtration and dried to obtain 11.19 g of the title compound (Yield: 33.7%).

1. additionwas added dropwise over 5 minutes
2. temperatureunder reflux for 1 hour
3. concentrationfollowed by concentration
4. customThe residue obtained
5. washwashed with water
6. dry with materialby drying over anhydrous magnesium sulfate
7. customThe solvent was evaporated
8. additionn-hexane was added to the set residue
9. filtrationThe crystals were collected by filtration
10. customdried