反应详情

温度

80 °C

To a mixture of 153 mg (5-bromo-thiophen-2-yl)-methanol, 128 mg pyridine-3-boronic acid, and 64 mg tetrakis(triphenylphosphine) palladium was added solvent (7.3 mL toluene and 3.1 mL methanol) followed by 1.4 mL of 2.5M sodium carbonate and the mixture heated to 80° C. on an oil bath. After 16 hours the mixture was cooled to room temperature and cocncentrated in vacuo. The residue was solvated in ethyl acetate was washed sequentially with 0.5N sodium hydroxide and brine, dried over magnesium sulfate and concentrated in vacuo. Purification by flash chromatography on silica gel (hexane:ethyl acetate, 60:40; then 55:45) gave the title compound (147 mg).

1. temperatureAfter 16 hours the mixture was cooled to room temperature
2. washwas washed sequentially with 0.5N sodium hydroxide and brine
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated in vacuo
5. customPurification by flash chromatography on silica gel (hexane