反应详情

温度

80 °C

Mix 3-[3-(2-bromo-ethoxy)-phenyl]-thieno[2,3-d]isoxazole (0.40 g, 1.23 mmol), potassium carbonate (0.341 g, 2.47 mmol), 2-fluorobenzylamine (0.626 g, 5.0 mmol) and acetonitrile (5.0 mL) and heat at 80° C., overnight. Cool the reaction mixture and filter through a Waters Sep-Pak 1 g silica cartridge (ethyl acetate). Combine the appropriate fractions and concentrate to give a residue. Purify the residue by column (10 g silica) chromatography using a solvent gradient of 40% ethyl acetate in heptane to 100% ethyl acetate to obtain the title compound (0.378 g, 83% Yield). Purity by LC/MS (APCI)=99%, [M+H]+=369.

1. temperatureCool the reaction mixture
2. filtrationfilter through a Waters Sep-Pak 1 g silica cartridge (ethyl acetate)
3. concentrationCombine the appropriate fractions and concentrate
4. customto give a residue
5. customPurify the residue by column (10 g silica) chromatography