反应详情

温度

120 °C

To a solution of 5-(4-fluoro-phenyl)-3-methyl-3H-[1,2,3]triazole-4-carbaldehyde (308 mg, 1.5 mmol) in acetic anhydride (0.8 mL) and AcOH (141 μL) was added methyl-6-methylnicotinate (227 mg, 1.5 mmol) and the reaction mixture was heated at 120° C. for 144 h. The mixture was then poured into water, sodium hydroxide (2 N) added and extracted with ethyl acetate and the combined organic extracts washed with brine, dried over sodium sulphate, filtered and evaporated. Purification by chromatography (silica, 0 to 10% methanol in dichloromethane) afforded the title compound (154 mg, 30%) as a light brown solid. MS: m/e=339.1 [M+H]+.

1. additionadded
2. extractionextracted with ethyl acetate
3. washthe combined organic extracts washed with brine
4. dry with materialdried over sodium sulphate
5. filtrationfiltered
6. customevaporated
7. customPurification by chromatography (silica, 0 to 10% methanol in dichloromethane)