反应详情

温度

110 °C

5.00 g (23.6 mMol) of 3,5-diethoxy-4-fluoro-benzaldehyde (example 50 g), 3.25 g (=2.0 eq.) of 1,2,4-triazole and 6.51 g (=2.0 eq.) of potassium carbonate was dissolved under argon in 50 mL of DMSO; the reaction mixture was stirred for 1 hour at 110° C. Then, it was cooled down to ambient temperature, poured into crashed ice and extracted twice with ethyl acetate. The organic phases were washed with water, dried over MgSO4, filtered and evaporated i.V. The crude product was purified by chromatography (silicagel, eluent:gradient of n-heptane/ethyl acetate) to yield 5.28 g of the title compound as colorless solid. MS: 261.9 (MH+).

1. temperatureThen, it was cooled down to ambient temperature
2. additionpoured
3. extractionextracted twice with ethyl acetate
4. washThe organic phases were washed with water
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customevaporated i.V
8. customThe crude product was purified by chromatography (silicagel, eluent:gradient of n-heptane/ethyl acetate)