反应详情

温度

110 °C

To a solution of 3,5-diethoxy-4-fluoro-benzaldehyde (5.00 g, 23.56 mmol, 1.0 equiv; intermediate 21) in DMSO (50 mL) was added 1H-[1,2,4]triazole (3.26 g, 47.12 mmol, 2.0 equiv) and K2CO3 (6.51 g, 47.12 mmol, 2.0 equiv) and the reaction mixture stirred at 110° C. for 1 h. The solution was poured on crashed ice, the reaction mixture extracted with ethyl acetate (2×50 mL) and the combined organic phases dried over MgSO4. The organic solvent was evaporated under reduced pressure and the crude reaction product purified with column chromatography on silica eluting with a gradient of heptane/ethyl acetate (1:1→0:1) providing 5.28 g (86%) of the title compound. MS (ESI): 261.9 [M+H]+.

1. additionThe solution was poured
2. extractionthe reaction mixture extracted with ethyl acetate (2×50 mL)
3. dry with materialthe combined organic phases dried over MgSO4
4. customThe organic solvent was evaporated under reduced pressure
5. customthe crude reaction product
6. custompurified with column chromatography on silica eluting with a gradient of heptane/ethyl acetate (1:1→0:1)