反应详情

温度

90 °C

A mixture of 4-chloro-2-(methylthio)pyrimidine (3 g, 18.7 mmol), 4-chloro-phenylboronic acid (3.5 g, 22.3 mmol), tetrakis(triphenylphosphine)palladium (0) (0.43 g, 0.37 mmol), sodium carbonate (5.15 g, 48.5 mmol) in 1,2-dimethoxyethane (140 mL) and water (70 mL) was heated at 90° C. for 20 h under nitrogen. The cooled reaction mixture was concentrated In vacuo, diluted with water (50 mL), extracted with CH2Cl2 (2×100 ml), dried (Na2SO4) and the solvent removed in vacuo. Purification by Biotage™ chromatography (silica, 90 g) eluting with 10:1 to 2:1 cyclohexane:EtOAc afforded the title compound as a white solid (3.98 g).

1. customThe cooled reaction mixture
2. concentrationwas concentrated In vacuo
3. additiondiluted with water (50 mL)
4. extractionextracted with CH2Cl2 (2×100 ml)
5. dry with materialdried (Na2SO4)
6. customthe solvent removed in vacuo
7. customPurification by Biotage™ chromatography (silica, 90 g)
8. washeluting with 10:1 to 2:1 cyclohexane