反应详情

温度

68 °C

3-Bromo-2-methyl-6-(4H-1,2,4-triazol-3-yl)pyridine (1 equiv), 3,4-dihydro-2H-pyran (2 equiv) and methanesulfonic acid (0.1 equiv) were combined in tetrahydrofuran. The reaction was heated to 68° C. for 3.5 h, cooled to room temperature, and treated with triethylamine (0.4 equiv). The reaction mixture was concentrated under reduced pressure, treated with acetonitrile and concentrated under reduced pressure at 35° C. The residue was dissolved in acetonitrile (1 volume) and water (2.25 volumes), and the solids were collected by filtration, washed with a solution of 20% acetonitrile in water and dried. The crude product was triturated with hexanes, filtered, washed with hexanes and dried to provide the desired product, as a solid. MS (ESI) m/z 324.9 [M+2]+.

1. temperaturecooled to room temperature
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. additiontreated with acetonitrile
4. concentrationconcentrated under reduced pressure at 35° C
5. dissolutionThe residue was dissolved in acetonitrile (1 volume)
6. filtrationwater (2.25 volumes), and the solids were collected by filtration
7. washwashed with a solution of 20% acetonitrile in water
8. customdried
9. customThe crude product was triturated with hexanes
10. filtrationfiltered
11. washwashed with hexanes
12. customdried