反应详情

温度

130 °C

A resealable pressure bottle was charged with 4-(2-chloropyridin-3-yl)-2-(methylthio)pyrimidine (6.00 g, 25.2 mmol), 4-aminophenol (2.89 g, 26.5 mmol), and cesium carbonate (16.4 g, 50.5 mmol). These reagents were suspended in DMSO (50.5 ml, 0.50 M). The vessel was sealed and heated to 130° C. for 48 hrs. Reaction mixture was allowed to cool to RT, diluted with water and extracted with EtOAc. The organic layer was collected, dried with Na2SO4, filtered, and concentrated to give a light brown residue, which was purified by silica gel chromatography (ISCO, 10% to 50% Ethyl Acetate/Hexanes) to afford clean material as light yellow solid. MS m/z=311 [M+H]+. Calc'd for C16H14N4OS: 310.37.

1. customThe vessel was sealed
2. customReaction mixture
3. temperatureto cool to RT
4. extractionextracted with EtOAc
5. customThe organic layer was collected
6. dry with materialdried with Na2SO4
7. filtrationfiltered
8. concentrationconcentrated
9. customto give a light brown residue, which
10. customwas purified by silica gel chromatography (ISCO, 10% to 50% Ethyl Acetate/Hexanes)
11. customto afford clean material as light yellow solid