反应详情

A solution of 1-(1-(2-fluorophenyl)-4-methyl-1H-1,2,3-triazol-5-yl)ethanone (1.66 g, 7.57 mmol) was dissolved in chloroform (12 mL) and acetic (0.24 mL) was heated to reflux and then a solution of bromine (0.41 mL, 7.95 mmol) in chloroform (5 mL) and heated under reflux for 2 h and then bromine (0.12 mL, 2.27 mmol) in chloroforom (2 mL) was added and heated under reflux for a further 30 min. After cooling to room temperature the mixture was poured onto ice-water and the mixture extracted with dichloromethane. The combined organic extracts were washed with water, brine, dried over sodium sulphate, filtered and evaporated. Purification by chromatography (silica, 10 to 60% ethyl acetate in heptane) afforded the title compound (1.54 g, 64%) as an off white solid. MS: m/e=298.1/300.0 [M+H]+.

1. temperatureto reflux
2. temperatureunder reflux for 2 h
3. temperatureheated
4. temperatureunder reflux for a further 30 min
5. additionwas poured onto ice-water
6. extractionthe mixture extracted with dichloromethane
7. washThe combined organic extracts were washed with water, brine
8. dry with materialdried over sodium sulphate
9. filtrationfiltered
10. customevaporated
11. customPurification by chromatography (silica, 10 to 60% ethyl acetate in heptane)