反应详情

A solution of 3-(4-Bromophenyl)-4H-1,2,4-triazole (14.1 g, 62.9 mmol), 3,4-dihydro-2H-pyran (10.59 mmol) and methanesulfonic acid (1.19 g, 6.29 mmol) in tetrahydrofuran (150 mL) was heated at 75° C. for 2 h. The solution was condensed and partitioned between sodium bicarbonate solution and ethyl acetate (3×), the organics dried over magnesium sulfate, filtered and solvent removed under reduced pressure. The solid was triturated with 10% ethyl acetate in hexanes to afford the title compound (8.1 g, 26.3 mmol, 70% yield). MS (ESI) m/z 308.4 [M]+, 310.5 [M+2]+.

1. customcondensed
2. custompartitioned between sodium bicarbonate solution and ethyl acetate (3×)
3. dry with materialthe organics dried over magnesium sulfate
4. filtrationfiltered
5. customsolvent removed under reduced pressure
6. customThe solid was triturated with 10% ethyl acetate in hexanes