反应详情

温度

40 °C

5-(3-Hydroxypropyl)-1-{[4-(methyloxy)phenyl]methyl}-1,2-dihydro-3,6-pyridazinedione (2.734 g) was treated with anisole (10 ml) and TFA (100 ml) and stirred at 40° C. overnight. The solution was cooled, evaporated to dryness and kept under high vacuum for 30 minutes. The residue was taken up in methanol (150 ml), refluxed for 12 hours, cooled and evaporated. The residue was kept 1 hour under high vacuum, triturated under ether and the solid filtered off. Drying under vacuum gave the product as a solid (1.48 g, 92%).

1. temperatureThe solution was cooled
2. customevaporated to dryness
3. waitkept under high vacuum for 30 minutes
4. temperaturerefluxed for 12 hours
5. temperaturecooled
6. customevaporated
7. waitThe residue was kept 1 hour under high vacuum
8. customtriturated under ether
9. filtrationthe solid filtered off
10. customDrying under vacuum