反应详情

温度

120 °C

A mixture of 5-methyl-2H-1,2,4-triazol-3-amine (147 mg, 1.50 mmol, 1.00 equiv), acetic acid (3 mL), and ethyl 3-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)-3-oxopropanoate (375 mg, 1.50 mmol, 1.00 equiv) was stirred for 16 hr at 120° C., then concentrated to dryness. The resulting solid was washed by 5 mL MeOH and collected by filtration. The solid was dissolved in 10 mL of NH4OH (aq.) and filtered. The filtrate was adjusted to pH<5 with HOAc, then concentrated to dryness. The resulting solid was washed by 10 mL water, collected by filtration, and dried to get 50 mg (12%) of 5-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)-2-methyl-[1,2,4]triazolo[1,5-α]pyrimidin-7(4H)-one as a yellow solid.

1. concentrationconcentrated to dryness
2. washThe resulting solid was washed by 5 mL MeOH
3. filtrationcollected by filtration
4. dissolutionThe solid was dissolved in 10 mL of NH4OH (aq.)
5. filtrationfiltered
6. concentrationconcentrated to dryness
7. washThe resulting solid was washed by 10 mL water
8. filtrationcollected by filtration
9. customdried