反应详情

温度

110 °C

A mixture of 5-trifluoromethyl-pyridine-2-thiol (6.99 g, 39.0 mmol), 4-fluorobenzaldehyde (4.79 g, 38.6 mmol), anhydrous K2CO3 (8.16 g, 59.1 mmol) and DMF (70 mL) was heated at 110° C. for 18 h. The mixture was cooled to room temperature and partitioned between MTBE and water. The phases were separated. The organic extracts were combined, dried over Na2SO4, filtered and evaporated to give a crude product which was purified by flash column chromatography (eluent: 5% MTBE in petroleum ether). Evaporation of the appropriate fractions gave the product (9.47 g, 87% yield). 1H NMR (CDCl3) δ 10.06 (s, 1H), 8.69-8.66 (m, 1H), 7.97-7.92 (m, 2H), 7.78-7.72 (m, 3H), 7.23-7.16 (m, 1H).

1. temperatureThe mixture was cooled to room temperature
2. custompartitioned between MTBE and water
3. customThe phases were separated
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. customevaporated
7. customto give a crude product which
8. customwas purified by flash column chromatography (eluent: 5% MTBE in petroleum ether)
9. customEvaporation of the appropriate fractions