反应详情

[4-(3-Bromo-5-hydroxy-phenylsulfanyl)-2-methyl-phenoxy]-acetic acid ethyl acetate (2.3 g; 5.79 mmol), phenylacetylene (1.9 mL; 17.4 mmol), bis(triphenylphosphine)palladium (II) chloride (0.33 g; 0.46 mmol) and copper iodide (0.07 g; 0.35 mmol) were dissolved in a mixture of triethylamine (7 mL) and DMF (8 mL) under an atmosphere of nitrogen. The reaction mixture was reacted in a microwave oven at 100° C. for 1 h. The reaction mixture was evaporated to dryness, and 5% aqueous citric acid and ethyl acetate was added. The organic phase was separated, dried and evaporated to dryness. The crude product was purified by flash chromatography (ethyl acetate:heptane 1:10→1:3). Yield: 1.2 g. HPLC-MS: m/z: 419 (M+); Rt: 2.52 min.

1. customThe reaction mixture was reacted in a microwave oven at 100° C. for 1 h
2. customThe reaction mixture was evaporated to dryness, and 5% aqueous citric acid and ethyl acetate
3. additionwas added
4. customThe organic phase was separated
5. customdried
6. customevaporated to dryness
7. customThe crude product was purified by flash chromatography (ethyl acetate:heptane 1:10→1:3)